CEP-37440_COA_11947_MedChemExpress
超高效液相色谱-串联质谱法测定人血浆中精氨酸及衍生物含量
超高效液相色谱-串联质谱法测定人血浆中精氨酸及衍生物含量田晔;江骥;胡蓓;薛金萍;王洪允【摘要】建立了超高效液相色谱-串联质谱(UPLC-MS/MS)法同时测定使用艾普拉唑后人血浆中二甲基精氨酸(ADMA)、对称二甲基精氨酸(SDMA)、单甲基精氨酸(NMMA)、瓜氨酸(Cit)和L-精氨酸(L-Arg)的浓度.采用HILIC亲水相互作用色谱和非衍生化的蛋白沉淀法进行分离分析,色谱柱选取Waters Atlantic HILIC柱(2.1 mm×50 mm×3μm),流动相由乙腈(含0.5％乙酸和0.025％三氟乙酸)-水(含0.5％乙酸和0.025％三氟乙酸)(85:15,v/V)组成,流速0.25 mL/min.采用多反应离子监测(MRM)模式,以电喷雾离子源(ESI)正离子方式检测.结果显示,ADMA、SDMA、NMMA、L-Arg和Cit的线性关系良好,相关系数r均大于0.994 0;ADMA、SDMA和NMMA的线性范围为0.1～5 mmol/L,L-Arg和Cit的线性范围为10～250 mmol/L;5种氨基酸的日内、日间精密度均小于15％,准确度在85％～115％之间.该方法快速、简便、灵敏,可为相关疾病的临床诊断提供一种高效的检测手段.【期刊名称】《质谱学报》【年(卷),期】2016(037)005【总页数】7页(P446-452)【关键词】超高效液相色谱-串联质谱(UPLC-MS/MS);艾普拉唑;蛋白沉淀法;亲水性色谱【作者】田晔;江骥;胡蓓;薛金萍;王洪允【作者单位】福州大学化学学院,福建省功能材料工程研究中心,福建省光动力治疗药物与诊疗工程技术研究中心,福建福州350108;中国医学科学院北京协和医院临床药理中心,北京100730;中国医学科学院北京协和医院临床药理中心,北京100730;中国医学科学院北京协和医院临床药理中心,北京100730;福州大学化学学院,福建省功能材料工程研究中心,福建省光动力治疗药物与诊疗工程技术研究中心,福建福州350108;中国医学科学院北京协和医院临床药理中心,北京100730【正文语种】中文【中图分类】O657.63一氧化氮是人体重要的信使分子，L-精氨酸(L-Arg)在一氧化氮全酶(NOS)的催化下，产生一氧化氮(NO)和瓜氨酸(Cit)[1-2]。
超高效液相色谱法测定辛伐他汀胶囊中叔丁基-4-羟基茴香醚与2,6-二叔丁基对甲酚的含量
超高效液相色谱法测定辛伐他汀胶囊中叔丁基-4-羟基茴香醚与2,6-二叔丁基对甲酚的含量张红;李婕;王学涛【摘要】Objective To establish a method for analysis of butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) in Simvastatin Capsules. Methods The chromatographic conditions included ACQUITY UPLCTM BEH C18 column (50 mm X 2. 1 mm, 1. 7 μm) ,mobile phase of acetonitrile(B) ;0. 005 mol o L-1 ammonium acetate(A) with gradient elution:0 min,60 : 40 ;2 min, 60 = 40; 5 min, 90 = 10; 8 min, 90 = 10; 9 min, 60 = 40; 10 min, 60 = 40 at a flow rate of 0. 25 mL o min-1 , the detection wavelength 280 nm,and the column temperature 40 °C. Results Good resolution for BHA,BHT and vitamin C was obtained. The limit of detection for BHA was 0. 5 ng,the linear range was 0. 203 5-50. 88 μg o mL-1 (r=0. 999 9) ,and the average recovery was 98. 3% (RSD=1. 0%). The limit of detection for BHT was 0. 5 ng.the linear range was 0. 211 4-52. 84 μg o mL-1 (r=0. 999 9) ,and the average recovery was 97. 2%(RSD=0. 5%). Conclusion The method is rapid,specific,sensitive and economic.%目的建立超高效液相色谱法同时测定辛伐他汀胶囊中的抗氧剂叔丁基-4-羟基茴香醚(BHA)与2,6-二叔丁基对甲酚(BHT).方法色谱柱为ACQUITY UPLCTM BEH C18 (50 mm×2.1 mm,1.7 μm).以乙腈(A)-0.005 mol·L-1醋酸铵(B)为流动相,梯度洗脱程序为:0 min,60∶40;2 min,60∶40;5 min,90∶10;8 min,90∶10;9 min,60∶40;10 min,60∶40.检测波长为280 nm,流速为0.25 mL·m in-1,柱温为40 ℃.结果在该色谱条件下,BHA和BHT与维生素C峰均能良好分离.BHA的检出限为0.5 ng;质量浓度在0.203 5～50.88 μg·mL-1范围内与峰面积呈良好的线性关系,相关系数r=0.999 9;回收率为98.3%,RSD为1.0%.BHT的检出限为0.5 ng;质量浓度在0.211 4～52.84 μg·mL-1范围内与峰面积呈良好的线性关系,相关系数r=0.999 9;回收率为97.2%,RSD为0.5%.结论该方法快速、专属、灵敏度高,并且节能环保.【期刊名称】《西北药学杂志》【年(卷),期】2012(027)005【总页数】3页(P420-422)【关键词】超高效液相色谱法;辛伐他汀;BHA;BHT【作者】张红;李婕;王学涛【作者单位】中国食品药品检定研究院,北京,100050;中国食品药品检定研究院,北京,100050;秦皇岛市药品检验所,秦皇岛,053000【正文语种】中文【中图分类】R927.2辛伐他汀是唯一列入国家基本药物目录的调脂及抗动脉粥样硬化药，国内有多家企业生产，由于其结构中的4－羟基－2 H－吡喃环易氧化，故常在制剂处方中加入抗氧剂以提高其稳定性，其中叔丁基－4－羟基茴香醚（BHA）和2，6－二叔丁基对甲酚（BHT）是最为常用的2种抗氧剂。
Gelucire-14-44-SDS-MedChemExpress
Inhibitors, Agonists, Screening LibrariesSafety Data Sheet Revision Date:Nov.-23-2018Print Date:Nov.-23-20181. PRODUCT AND COMPANY IDENTIFICATION1.1 Product identifierProduct name :Gelucire 14/44Catalog No. :HY-Y1892CAS No. :121548-04-71.2 Relevant identified uses of the substance or mixture and uses advised againstIdentified uses :Laboratory chemicals, manufacture of substances.1.3 Details of the supplier of the safety data sheetCompany:MedChemExpress USATel:609-228-6898Fax:609-228-5909E-mail:sales@1.4 Emergency telephone numberEmergency Phone #:609-228-68982. HAZARDS IDENTIFICATION2.1 Classification of the substance or mixtureNot a hazardous substance or mixture.2.2 GHS Label elements, including precautionary statementsNot a hazardous substance or mixture.2.3 Other hazardsNone.3. COMPOSITION/INFORMATION ON INGREDIENTS3.1 SubstancesSynonyms:NoneFormula:N/AMolecular Weight:N/ACAS No. :121548-04-74. FIRST AID MEASURES4.1 Description of first aid measuresEye contactRemove any contact lenses, locate eye-wash station, and flush eyes immediately with large amounts of water. Separate eyelids with fingers to ensure adequate flushing. Promptly call a physician.Skin contactRinse skin thoroughly with large amounts of water. Remove contaminated clothing and shoes and call a physician.InhalationImmediately relocate self or casualty to fresh air. If breathing is difficult, give cardiopulmonary resuscitation (CPR). Avoid mouth-to-mouth resuscitation.IngestionWash out mouth with water; Do NOT induce vomiting; call a physician.4.2 Most important symptoms and effects, both acute and delayedThe most important known symptoms and effects are described in the labelling (see section 2.2).4.3 Indication of any immediate medical attention and special treatment neededTreat symptomatically.5. FIRE FIGHTING MEASURES5.1 Extinguishing mediaSuitable extinguishing mediaUse water spray, dry chemical, foam, and carbon dioxide fire extinguisher.5.2 Special hazards arising from the substance or mixtureDuring combustion, may emit irritant fumes.5.3 Advice for firefightersWear self-contained breathing apparatus and protective clothing.6. ACCIDENTAL RELEASE MEASURES6.1 Personal precautions, protective equipment and emergency proceduresUse full personal protective equipment. Avoid breathing vapors, mist, dust or gas. Ensure adequate ventilation. Evacuate personnel to safe areas.Refer to protective measures listed in sections 8.6.2 Environmental precautionsTry to prevent further leakage or spillage. Keep the product away from drains or water courses.6.3 Methods and materials for containment and cleaning upAbsorb solutions with finely-powdered liquid-binding material (diatomite, universal binders); Decontaminate surfaces and equipment by scrubbing with alcohol; Dispose of contaminated material according to Section 13.7. HANDLING AND STORAGE7.1 Precautions for safe handlingAvoid inhalation, contact with eyes and skin. Avoid dust and aerosol formation. Use only in areas with appropriate exhaust ventilation.7.2 Conditions for safe storage, including any incompatibilitiesKeep container tightly sealed in cool, well-ventilated area. Keep away from direct sunlight and sources of ignition.Recommended storage temperature:Pure form-20°C 3 years4°C 2 yearsIn solvent-80°C 6 months-20°C 1 monthShipping at room temperature if less than 2 weeks.7.3 Specific end use(s)No data available.8. EXPOSURE CONTROLS/PERSONAL PROTECTION8.1 Control parametersComponents with workplace control parametersThis product contains no substances with occupational exposure limit values.8.2 Exposure controlsEngineering controlsEnsure adequate ventilation. Provide accessible safety shower and eye wash station.Personal protective equipmentEye protection Safety goggles with side-shields.Hand protection Protective gloves.Skin and body protection Impervious clothing.Respiratory protection Suitable respirator.Environmental exposure controls Keep the product away from drains, water courses or the soil. Cleanspillages in a safe way as soon as possible.9. PHYSICAL AND CHEMICAL PROPERTIES9.1 Information on basic physical and chemical propertiesAppearance White to off-white (Oil)Odor No data availableOdor threshold No data availablepH No data availableMelting/freezing point No data availableBoiling point/range No data availableFlash point No data availableEvaporation rate No data availableFlammability (solid, gas)No data availableUpper/lower flammability or explosive limits No data availableVapor pressure No data availableVapor density No data availableRelative density No data availableWater Solubility No data availablePartition coefficient No data availableAuto-ignition temperature No data availableDecomposition temperature No data availableViscosity No data availableExplosive properties No data availableOxidizing properties No data available9.2 Other safety informationNo data available.10. STABILITY AND REACTIVITY10.1 ReactivityNo data available.10.2 Chemical stabilityStable under recommended storage conditions.10.3 Possibility of hazardous reactionsNo data available.10.4 Conditions to avoidNo data available.10.5 Incompatible materialsStrong acids/alkalis, strong oxidising/reducing agents.10.6 Hazardous decomposition productsUnder fire conditions, may decompose and emit toxic fumes.Other decomposition products - no data available.11.TOXICOLOGICAL INFORMATION11.1 Information on toxicological effectsAcute toxicityClassified based on available data. For more details, see section 2Skin corrosion/irritationClassified based on available data. For more details, see section 2Serious eye damage/irritationClassified based on available data. For more details, see section 2Respiratory or skin sensitizationClassified based on available data. For more details, see section 2Germ cell mutagenicityClassified based on available data. For more details, see section 2CarcinogenicityIARC: No component of this product present at a level equal to or greater than 0.1% is identified as probable, possible or confirmed human carcinogen by IARC.ACGIH: No component of this product present at a level equal to or greater than 0.1% is identified as a potential or confirmed carcinogen by ACGIH.NTP: No component of this product present at a level equal to or greater than 0.1% is identified as a anticipated or confirmed carcinogen by NTP.OSHA: No component of this product present at a level equal to or greater than 0.1% is identified as a potential or confirmed carcinogen by OSHA.Reproductive toxicityClassified based on available data. For more details, see section 2Specific target organ toxicity - single exposureClassified based on available data. For more details, see section 2Specific target organ toxicity - repeated exposureClassified based on available data. For more details, see section 2Aspiration hazardClassified based on available data. For more details, see section 212. ECOLOGICAL INFORMATION12.1 ToxicityNo data available.12.2 Persistence and degradabilityNo data available.12.3 Bioaccumlative potentialNo data available.12.4 Mobility in soilNo data available.12.5 Results of PBT and vPvB assessmentPBT/vPvB assessment unavailable as chemical safety assessment not required or not conducted.12.6 Other adverse effectsNo data available.13. DISPOSAL CONSIDERATIONS13.1 Waste treatment methodsProductDispose substance in accordance with prevailing country, federal, state and local regulations.Contaminated packagingConduct recycling or disposal in accordance with prevailing country, federal, state and local regulations.14. TRANSPORT INFORMATIONDOT (US)This substance is considered to be non-hazardous for transport.IMDGThis substance is considered to be non-hazardous for transport.IATAThis substance is considered to be non-hazardous for transport.15. REGULATORY INFORMATIONSARA 302 Components:No chemicals in this material are subject to the reporting requirements of SARA Title III, Section 302.SARA 313 Components:This material does not contain any chemical components with known CAS numbers that exceed the threshold (De Minimis) reporting levels established by SARA Title III, Section 313.SARA 311/312 Hazards:No SARA Hazards.Massachusetts Right To Know Components:No components are subject to the Massachusetts Right to Know Act.Pennsylvania Right To Know Components:No components are subject to the Pennsylvania Right to Know Act.New Jersey Right To Know Components:No components are subject to the New Jersey Right to Know Act.California Prop. 65 Components:This product does not contain any chemicals known to State of California to cause cancer, birth defects, or anyother reproductive harm.16. OTHER INFORMATIONCopyright 2018 MedChemExpress. The above information is correct to the best of our present knowledge but does not purport to be all inclusive and should be used only as a guide. The product is for research use only and for experienced personnel. It must only be handled by suitably qualified experienced scientists in appropriately equipped and authorized facilities. The burden of safe use of this material rests entirely with the user. MedChemExpress disclaims all liability for any damage resulting from handling or from contact with this product.Caution: Product has not been fully validated for medical applications. For research use only.Tel: 609-228-6898 Fax: 609-228-5909 E-mail: tech@Address: 1 Deer Park Dr, Suite Q, Monmouth Junction, NJ 08852, USA。
稳定性英文版
HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationFLUOXETINE HClC17H18F3NO•HClM.W. = 345.79CAS — 59333-67-4STABILITY INDICATINGA S S A Y V A L I D A T I O NMethod is suitable for:ýIn-process controlþProduct ReleaseþStability indicating analysis (Suitability - US/EU Product) CAUTIONFLUOXETINE HYDROCHLORIDE IS A HAZARDOUS CHEMICAL AND SHOULD BE HANDLED ONLY UNDER CONDITIONS SUITABLE FOR HAZARDOUS WORK.IT IS HIGHLY PRESSURE SENSITIVE AND ADEQUATE PRECAUTIONS SHOULD BE TAKEN TO AVOID ANY MECHANICAL FORCE (SUCH AS GRINDING, CRUSHING, ETC.) ON THE POWDER.ED. N0: 04Effective Date:APPROVED::HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationTABLE OF CONTENTS INTRODUCTION........................................................................................................................ PRECISION............................................................................................................................... System Repeatability ................................................................................................................ Method Repeatability................................................................................................................. Intermediate Precision .............................................................................................................. LINEARITY................................................................................................................................ RANGE...................................................................................................................................... ACCURACY............................................................................................................................... Accuracy of Standard Injections................................................................................................ Accuracy of the Drug Product.................................................................................................... VALIDATION OF FLUOXETINE HCl AT LOW CONCENTRATION........................................... Linearity at Low Concentrations................................................................................................. Accuracy of Fluoxetine HCl at Low Concentration..................................................................... System Repeatability................................................................................................................. Quantitation Limit....................................................................................................................... Detection Limit........................................................................................................................... VALIDATION FOR META-FLUOXETINE HCl (POSSIBLE IMPURITIES).................................. Meta-Fluoxetine HCl linearity at 0.05% - 1.0%........................................................................... Detection Limit for Fluoxetine HCl.............................................................................................. Quantitation Limit for Meta Fluoxetine HCl................................................................................ Accuracy for Meta-Fluoxetine HCl ............................................................................................ Method Repeatability for Meta-Fluoxetine HCl........................................................................... Intermediate Precision for Meta-Fluoxetine HCl......................................................................... SPECIFICITY - STABILITY INDICATING EVALUATION OF THE METHOD............................. FORCED DEGRADATION OF FINISHED PRODUCT AND STANDARD..................................1. Unstressed analysis...............................................................................................................2. Acid Hydrolysis stressed analysis..........................................................................................3. Base hydrolysis stressed analysis.........................................................................................4. Oxidation stressed analysis...................................................................................................5. Sunlight stressed analysis.....................................................................................................6. Heat of solution stressed analysis.........................................................................................7. Heat of powder stressed analysis.......................................................................................... System Suitability stressed analysis.......................................................................................... Placebo...................................................................................................................................... STABILITY OF STANDARD AND SAMPLE SOLUTIONS......................................................... Standard Solution...................................................................................................................... Sample Solutions....................................................................................................................... ROBUSTNESS.......................................................................................................................... Extraction................................................................................................................................... Factorial Design......................................................................................................................... CONCLUSION...........................................................................................................................ED. N0: 04Effective Date:APPROVED::HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationBACKGROUNDTherapeutically, Fluoxetine hydrochloride is a classified as a selective serotonin-reuptake inhibitor. Effectively used for the treatment of various depressions. Fluoxetine hydrochloride has been shown to have comparable efficacy to tricyclic antidepressants but with fewer anticholinergic side effects. The patent expiry becomes effective in 2001 (US). INTRODUCTIONFluoxetine capsules were prepared in two dosage strengths: 10mg and 20mg dosage strengths with the same capsule weight. The formulas are essentially similar and geometrically equivalent with the same ingredients and proportions. Minor changes in non-active proportions account for the change in active ingredient amounts from the 10 and 20 mg strength.The following validation, for the method SI-IAG-206-02 , includes assay and determination of Meta-Fluoxetine by HPLC, is based on the analytical method validation SI-IAG-209-06. Currently the method is the in-house method performed for Stability Studies. The Validation was performed on the 20mg dosage samples, IAG-21-001 and IAG-21-002.In the forced degradation studies, the two placebo samples were also used. PRECISIONSYSTEM REPEATABILITYFive replicate injections of the standard solution at the concentration of 0.4242mg/mL as described in method SI-IAG-206-02 were made and the relative standard deviation (RSD) of the peak areas was calculated.SAMPLE PEAK AREA#15390#25406#35405#45405#55406Average5402.7SD 6.1% RSD0.1ED. N0: 04Effective Date:APPROVED::HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationED. N0: 04Effective Date:APPROVED::PRECISION - Method RepeatabilityThe full HPLC method as described in SI-IAG-206-02 was carried-out on the finished product IAG-21-001 for the 20mg dosage form. The method repeated six times and the relative standard deviation (RSD) was calculated.SAMPLENumber%ASSAYof labeled amountI 96.9II 97.8III 98.2IV 97.4V 97.7VI 98.5(%) Average97.7SD 0.6(%) RSD0.6PRECISION - Intermediate PrecisionThe full method as described in SI-IAG-206-02 was carried-out on the finished product IAG-21-001 for the 20mg dosage form. The method was repeated six times by a second analyst on a different day using a different HPLC instrument. The average assay and the relative standard deviation (RSD) were calculated.SAMPLENumber% ASSAYof labeled amountI 98.3II 96.3III 94.6IV 96.3V 97.8VI 93.3Average (%)96.1SD 2.0RSD (%)2.1The difference between the average results of method repeatability and the intermediate precision is 1.7%.HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationLINEARITYStandard solutions were prepared at 50% to 200% of the nominal concentration required by the assay procedure. Linear regression analysis demonstrated acceptability of the method for quantitative analysis over the concentration range required. Y-Intercept was found to be insignificant.RANGEDifferent concentrations of the sample (IAG-21-001) for the 20mg dosage form were prepared, covering between 50% - 200% of the nominal weight of the sample.Conc. (%)Conc. (mg/mL)Peak Area% Assayof labeled amount500.20116235096.7700.27935334099.21000.39734463296.61500.64480757797.52000.79448939497.9(%) Average97.6SD 1.0(%) RSD 1.0ED. N0: 04Effective Date:APPROVED::HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationED. N0: 04Effective Date:APPROVED::RANGE (cont.)The results demonstrate linearity as well over the specified range.Correlation coefficient (RSQ)0.99981 Slope11808.3Y -Interceptresponse at 100%* 100 (%) 0.3%ACCURACYACCURACY OF STANDARD INJECTIONSFive (5) replicate injections of the working standard solution at concentration of 0.4242mg/mL, as described in method SI-IAG-206-02 were made.INJECTIONNO.PEAK AREA%ACCURACYI 539299.7II 540599.9III 540499.9IV 5406100.0V 5407100.0Average 5402.899.9%SD 6.10.1RSD, (%)0.10.1The percent deviation from the true value wasdetermined from the linear regression lineHPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationED. N0: 04Effective Date:APPROVED::ACCURACY OF THE DRUG PRODUCTAdmixtures of non-actives (placebo, batch IAG-21-001 ) with Fluoxetine HCl were prepared at the same proportion as in a capsule (70%-180% of the nominal concentration).Three preparations were made for each concentration and the recovery was calculated.Conc.(%)Placebo Wt.(mg)Fluoxetine HCl Wt.(mg)Peak Area%Accuracy Average (%)70%7079.477.843465102.27079.687.873427100.77079.618.013465100.0101.0100%10079.6211.25476397.910080.8011.42491799.610079.6011.42485498.398.6130%13079.7214.90640599.413080.3114.75632899.213081.3314.766402100.399.618079.9920.10863699.318079.3820.45879499.418080.0820.32874899.599.4Placebo, Batch Lot IAG-21-001HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationED. N0: 04Effective Date:APPROVED::VALIDATION OF FLUOXETINE HClAT LOW CONCENTRATIONLINEARITY AT LOW CONCENTRATIONSStandard solution of Fluoxetine were prepared at approximately 0.02%-1.0% of the working concentration required by the method SI-IAG-206-02. Linear regression analysis demonstrated acceptability of the method for quantitative analysis over this range.ACCURACY OF FLUOXETINE HCl AT LOW CONCENTRATIONThe peak areas of the standard solution at the working concentration were measured and the percent deviation from the true value, as determined from the linear regression was calculated.SAMPLECONC.µg/100mLAREA FOUND%ACCURACYI 470.56258499.7II 470.56359098.1III 470.561585101.3IV 470.561940100.7V 470.56252599.8VI 470.56271599.5(%) AverageSlope = 132.7395299.9SD Y-Intercept = -65.872371.1(%) RSD1.1HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationSystem RepeatabilitySix replicate injections of standard solution at 0.02% and 0.05% of working concentration as described in method SI-IAG-206-02 were made and the relative standard deviation was calculated.SAMPLE FLUOXETINE HCl AREA0.02%0.05%I10173623II11503731III10103475IV10623390V10393315VI10953235Average10623462RSD, (%) 5.0 5.4Quantitation Limit - QLThe quantitation limit ( QL) was established by determining the minimum level at which the analyte was quantified. The quantitation limit for Fluoxetine HCl is 0.02% of the working standard concentration with resulting RSD (for six injections) of 5.0%. Detection Limit - DLThe detection limit (DL) was established by determining the minimum level at which the analyte was reliably detected. The detection limit of Fluoxetine HCl is about 0.01% of the working standard concentration.ED. N0: 04Effective Date:APPROVED::HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationED. N0: 04Effective Date:APPROVED::VALIDATION FOR META-FLUOXETINE HCl(EVALUATING POSSIBLE IMPURITIES)Meta-Fluoxetine HCl linearity at 0.05% - 1.0%Relative Response Factor (F)Relative response factor for Meta-Fluoxetine HCl was determined as slope of Fluoxetine HCl divided by the slope of Meta-Fluoxetine HCl from the linearity graphs (analysed at the same time).F =132.7395274.859534= 1.8Detection Limit (DL) for Fluoxetine HClThe detection limit (DL) was established by determining the minimum level at which the analyte was reliably detected.Detection limit for Meta Fluoxetine HCl is about 0.02%.Quantitation Limit (QL) for Meta-Fluoxetine HClThe QL is determined by the analysis of samples with known concentration of Meta-Fluoxetine HCl and by establishing the minimum level at which the Meta-Fluoxetine HCl can be quantified with acceptable accuracy and precision.Six individual preparations of standard and placebo spiked with Meta-Fluoxetine HCl solution to give solution with 0.05% of Meta Fluoxetine HCl, were injected into the HPLC and the recovery was calculated.HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationED. N0: 04Effective Date:APPROVED::META-FLUOXETINE HCl[RECOVERY IN SPIKED SAMPLES].Approx.Conc.(%)Known Conc.(µg/100ml)Area in SpikedSampleFound Conc.(µg/100mL)Recovery (%)0.0521.783326125.735118.10.0521.783326825.821118.50.0521.783292021.55799.00.0521.783324125.490117.00.0521.783287220.96996.30.0521.783328526.030119.5(%) AVERAGE111.4SD The recovery result of 6 samples is between 80%-120%.10.7(%) RSDQL for Meta Fluoxetine HCl is 0.05%.9.6Accuracy for Meta Fluoxetine HClDetermination of Accuracy for Meta-Fluoxetine HCl impurity was assessed using triplicate samples (of the drug product) spiked with known quantities of Meta Fluoxetine HCl impurity at three concentrations levels (namely 80%, 100% and 120% of the specified limit - 0.05%).The results are within specifications:For 0.4% and 0.5% recovery of 85% -115%For 0.6% recovery of 90%-110%HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationED. N0: 04Effective Date:APPROVED::META-FLUOXETINE HCl[RECOVERY IN SPIKED SAMPLES]Approx.Conc.(%)Known Conc.(µg/100mL)Area in spikedSample Found Conc.(µg/100mL)Recovery (%)[0.4%]0.4174.2614283182.66104.820.4174.2614606187.11107.370.4174.2614351183.59105.36[0.5%]0.5217.8317344224.85103.220.5217.8316713216.1599.230.5217.8317341224.81103.20[0.6%]0.6261.3918367238.9591.420.6261.3920606269.81103.220.6261.3920237264.73101.28RECOVERY DATA DETERMINED IN SPIKED SAMPLESHPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationED. N0: 04Effective Date:APPROVED::REPEATABILITYMethod Repeatability - Meta Fluoxetine HClThe full method (as described in SI-IAG-206-02) was carried out on the finished drug product representing lot number IAG-21-001-(1). The HPLC method repeated serially, six times and the relative standard deviation (RSD) was calculated.IAG-21-001 20mg CAPSULES - FLUOXETINESample% Meta Fluoxetine % Meta-Fluoxetine 1 in Spiked Solution10.0260.09520.0270.08630.0320.07740.0300.07450.0240.09060.0280.063AVERAGE (%)0.0280.081SD 0.0030.012RSD, (%)10.314.51NOTE :All results are less than QL (0.05%) therefore spiked samples with 0.05% Meta Fluoxetine HCl were injected.HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationED. N0: 04Effective Date:APPROVED::Intermediate Precision - Meta-Fluoxetine HClThe full method as described in SI-IAG-206-02 was applied on the finished product IAG-21-001-(1) .It was repeated six times, with a different analyst on a different day using a different HPLC instrument.The difference between the average results obtained by the method repeatability and the intermediate precision was less than 30.0%, (11.4% for Meta-Fluoxetine HCl as is and 28.5% for spiked solution).IAG-21-001 20mg - CAPSULES FLUOXETINESample N o:Percentage Meta-fluoxetine% Meta-fluoxetine 1 in spiked solution10.0260.06920.0270.05730.0120.06140.0210.05850.0360.05560.0270.079(%) AVERAGE0.0250.063SD 0.0080.009(%) RSD31.514.51NOTE:All results obtained were well below the QL (0.05%) thus spiked samples slightly greater than 0.05% Meta-Fluoxetine HCl were injected. The RSD at the QL of the spiked solution was 14.5%HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationSPECIFICITY - STABILITY INDICATING EVALUATIONDemonstration of the Stability Indicating parameters of the HPLC assay method [SI-IAG-206-02] for Fluoxetine 10 & 20mg capsules, a suitable photo-diode array detector was incorporated utilizing a commercial chromatography software managing system2, and applied to analyze a range of stressed samples of the finished drug product.GLOSSARY of PEAK PURITY RESULT NOTATION (as reported2):Purity Angle-is a measure of spectral non-homogeneity across a peak, i.e. the weighed average of all spectral contrast angles calculated by comparing all spectra in the integrated peak against the peak apex spectrum.Purity Threshold-is the sum of noise angle3 and solvent angle4. It is the limit of detection of shape differences between two spectra.Match Angle-is a comparison of the spectrum at the peak apex against a library spectrum.Match Threshold-is the sum of the match noise angle3 and match solvent angle4.3Noise Angle-is a measure of spectral non-homogeneity caused by system noise.4Solvent Angle-is a measure of spectral non-homogeneity caused by solvent composition.OVERVIEWT he assay of the main peak in each stressed solution is calculated according to the assay method SI-IAG-206-02, against the Standard Solution, injected on the same day.I f the Purity Angle is smaller than the Purity Threshold and the Match Angle is smaller than the Match Threshold, no significant differences between spectra can be detected. As a result no spectroscopic evidence for co-elution is evident and the peak is considered to be pure.T he stressed condition study indicated that the Fluoxetine peak is free from any appreciable degradation interference under the stressed conditions tested. Observed degradation products peaks were well separated from the main peak.1® PDA-996 Waters™ ; 2[Millennium 2010]ED. N0: 04Effective Date:APPROVED::HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationFORCED DEGRADATION OF FINISHED PRODUCT & STANDARD 1.UNSTRESSED SAMPLE1.1.Sample IAG-21-001 (2) (20mg/capsule) was prepared as stated in SI-IAG-206-02 and injected into the HPLC system. The calculated assay is 98.5%.SAMPLE - UNSTRESSEDFluoxetine:Purity Angle:0.075Match Angle:0.407Purity Threshold:0.142Match Threshold:0.4251.2.Standard solution was prepared as stated in method SI-IAG-206-02 and injected into the HPLC system. The calculated assay is 100.0%.Fluoxetine:Purity Angle:0.078Match Angle:0.379Purity Threshold:0.146Match Threshold:0.4272.ACID HYDROLYSIS2.1.Sample solution of IAG-21-001 (2) (20mg/capsule) was prepared as in method SI-IAG-206-02 : An amount equivalent to 20mg Fluoxetine was weighed into a 50mL volumetric flask. 20mL Diluent was added and the solution sonicated for 10 minutes. 1mL of conc. HCl was added to this solution The solution was allowed to stand for 18 hours, then adjusted to about pH = 5.5 with NaOH 10N, made up to volume with Diluent and injected into the HPLC system after filtration.Fluoxetine peak intensity did NOT decrease. Assay result obtained - 98.8%.SAMPLE- ACID HYDROLYSISFluoxetine peak:Purity Angle:0.055Match Angle:0.143Purity Threshold:0.096Match Threshold:0.3712.2.Standard solution was prepared as in method SI-IAG-206-02 : about 22mg Fluoxetine HCl were weighed into a 50mL volumetric flask. 20mL Diluent were added. 2mL of conc. HCl were added to this solution. The solution was allowed to stand for 18 hours, then adjusted to about pH = 5.5 with NaOH 10N, made up to volume with Diluent and injected into the HPLC system.Fluoxetine peak intensity did NOT decrease. Assay result obtained - 97.2%.ED. N0: 04Effective Date:APPROVED::HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationSTANDARD - ACID HYDROLYSISFluoxetine peak:Purity Angle:0.060Match Angle:0.060Purity Threshold:0.099Match Threshold:0.3713.BASE HYDROLYSIS3.1.Sample solution of IAG-21-001 (2) (20mg/capsule) was prepared as per method SI-IAG-206-02 : An amount equivalent to 20mg Fluoxetine was weight into a 50mL volumetric flask. 20mL Diluent was added and the solution sonicated for 10 minutes. 1mL of 5N NaOH was added to this solution. The solution was allowed to stand for 18 hours, then adjusted to about pH = 5.5 with 5N HCl, made up to volume with Diluent and injected into the HPLC system.Fluoxetine peak intensity did NOT decrease. Assay result obtained - 99.3%.SAMPLE - BASE HYDROLYSISFluoxetine peak:Purity Angle:0.063Match Angle:0.065Purity Threshold:0.099Match Threshold:0.3623.2.Standard stock solution was prepared as per method SI-IAG-206-02 : About 22mg Fluoxetine HCl was weighed into a 50mL volumetric flask. 20mL Diluent was added. 2mL of 5N NaOH was added to this solution. The solution was allowed to stand for 18 hours, then adjusted to about pH=5.5 with 5N HCl, made up to volume with Diluent and injected into the HPLC system.Fluoxetine peak intensity did NOT decrease - 99.5%.STANDARD - BASE HYDROLYSISFluoxetine peak:Purity Angle:0.081Match Angle:0.096Purity Threshold:0.103Match Threshold:0.3634.OXIDATION4.1.Sample solution of IAG-21-001 (2) (20mg/capsule) was prepared as per method SI-IAG-206-02. An equivalent to 20mg Fluoxetine was weighed into a 50mL volumetric flask. 20mL Diluent added and the solution sonicated for 10 minutes.1.0mL of 30% H2O2 was added to the solution and allowed to stand for 5 hours, then made up to volume with Diluent, filtered and injected into HPLC system.Fluoxetine peak intensity decreased to 95.2%.ED. N0: 04Effective Date:APPROVED::HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationSAMPLE - OXIDATIONFluoxetine peak:Purity Angle:0.090Match Angle:0.400Purity Threshold:0.154Match Threshold:0.4294.2.Standard solution was prepared as in method SI-IAG-206-02 : about 22mg Fluoxetine HCl were weighed into a 50mL volumetric flask and 25mL Diluent were added. 2mL of 30% H2O2 were added to this solution which was standing for 5 hours, made up to volume with Diluent and injected into the HPLC system.Fluoxetine peak intensity decreased to 95.8%.STANDARD - OXIDATIONFluoxetine peak:Purity Angle:0.083Match Angle:0.416Purity Threshold:0.153Match Threshold:0.4295.SUNLIGHT5.1.Sample solution of IAG-21-001 (2) (20mg/capsule) was prepared as in method SI-IAG-206-02 . The solution was exposed to 500w/hr. cell sunlight for 1hour. The BST was set to 35°C and the ACT was 45°C. The vials were placed in a horizontal position (4mm vials, National + Septum were used). A Dark control solution was tested. A 2%w/v quinine solution was used as the reference absorbance solution.Fluoxetine peak decreased to 91.2% and the dark control solution showed assay of 97.0%. The difference in the absorbance in the quinine solution is 0.4227AU.Additional peak was observed at RRT of 1.5 (2.7%).The total percent of Fluoxetine peak with the degradation peak is about 93.9%.SAMPLE - SUNLIGHTFluoxetine peak:Purity Angle:0.093Match Angle:0.583Purity Threshold:0.148Match Threshold:0.825 ED. N0: 04Effective Date:APPROVED::HPLC ASSAY with DETERMINATION OF META-FLUOXETINE HCl.ANALYTICAL METHOD VALIDATION10 and 20mg Fluoxetine Capsules HPLC DeterminationSUNLIGHT (Cont.)5.2.Working standard solution was prepared as in method SI-IAG-206-02 . The solution was exposed to 500w/hr. cell sunlight for 1.5 hour. The BST was set to 35°C and the ACT was 42°C. The vials were placed in a horizontal position (4mm vials, National + Septum were used). A Dark control solution was tested. A 2%w/v quinine solution was used as the reference absorbance solution.Fluoxetine peak was decreased to 95.2% and the dark control solution showed assay of 99.5%.The difference in the absorbance in the quinine solution is 0.4227AU.Additional peak were observed at RRT of 1.5 (2.3).The total percent of Fluoxetine peak with the degradation peak is about 97.5%. STANDARD - SUNLIGHTFluoxetine peak:Purity Angle:0.067Match Angle:0.389Purity Threshold:0.134Match Threshold:0.8196.HEAT OF SOLUTION6.1.Sample solution of IAG-21-001-(2) (20 mg/capsule) was prepared as in method SI-IAG-206-02 . Equivalent to 20mg Fluoxetine was weighed into a 50mL volumetric flask. 20mL Diluent was added and the solution was sonicated for 10 minutes and made up to volume with Diluent. 4mL solution was transferred into a suitable crucible, heated at 105°C in an oven for 2 hours. The sample was cooled to ambient temperature, filtered and injected into the HPLC system.Fluoxetine peak was decreased to 93.3%.SAMPLE - HEAT OF SOLUTION [105o C]Fluoxetine peak:Purity Angle:0.062Match Angle:0.460Purity Threshold:0.131Match Threshold:0.8186.2.Standard Working Solution (WS) was prepared under method SI-IAG-206-02 . 4mL of the working solution was transferred into a suitable crucible, placed in an oven at 105°C for 2 hours, cooled to ambient temperature and injected into the HPLC system.Fluoxetine peak intensity did not decrease - 100.5%.ED. N0: 04Effective Date:APPROVED::。
液相色谱-质谱联用测定抗风湿类中药中非法添加化学药物成分
时珍国医国药 ２０１０ 年第 ２１ 卷第 ４ 期
液 相 色 谱 －质 谱 联 用 测定抗风湿类中药中非法添加化学药物成分
来国防１ ， 程 宾１ ， 鲁 静２
（１．云南省食品药品检验所，云南 昆明 ６５００１１； ２．中国药品生物制品检定所，北京 １０００５０）
表 ２ 对照品标准曲线
对照品
回归方程
ｒ
线性范围 ／μｇ· ｍｌ －１
阿司匹林 氨基比林
布洛芬 双氯芬酸钠
吲哚美辛
Ｙ ＝２．９２ｅ ＋００４Ｘ ＋ １．３５ｅ ＋００５ Ｙ ＝９．００ｅ ＋００３ Ｘ － ２．４５ｅ ＋００２ Ｙ ＝５．２０ｅ ＋００４ Ｘ ＋ １．１０ｅ ＋００４ Ｙ ＝１．８３ｅ ＋００４ Ｘ ＋ ５．５７ｅ ＋００３ Ｙ ＝１．８２ｅ ＋００４ Ｘ ＋ ５．２４ｅ ＋００３
［ ４ ］ 周 艳，胡 琳，张宏祥，等．检查天麻胶囊中添加吲哚美辛的方法 研究［ Ｊ］ ．中国药事，２００６，２０（１０） ：６１２．
［ ５ ］ 马春燕，许 啸，冯益明，等．天麻胶囊中非法掺入西药吲哚美辛的 检出方法［ Ｊ］ ．中国药品标准，２００７，８（２） ：６６．
· ８４８· 万方数据
摘要：目的 建立快速、准确、高灵敏度的测定抗风湿类中药制剂中非法添加阿司匹林、氨基比林、布洛芬、双氯芬酸钠、吲
哚美辛分析方法。 方法 采用 ＨＰＬＣ －ＤＡＤ、ＵＰＬＣ ／ＭＳ ／ＭＳ 法对非法掺入的化学药物进行定性鉴别，并以 ＨＰＬＣ 测定含 量。 结果 受试制剂中检测到掺有氨基比林、布洛芬、双氯芬酸钠、吲哚美辛。 结论 此方法灵敏准确，可作为抗风湿类中 药制剂中非法添加阿司匹林、氨基比林、布洛芬、双氯芬酸钠、吲哚美辛的有效检测方法。
Pimecrolimus_SDS_MedChemExpress
Inhibitors, Agonists, Screening LibrariesSafety Data Sheet Revision Date:May-24-2017Print Date:May-24-20171. PRODUCT AND COMPANY IDENTIFICATION1.1 Product identifierProduct name :PimecrolimusCatalog No. :HY-13723CAS No. :137071-32-01.2 Relevant identified uses of the substance or mixture and uses advised againstIdentified uses :Laboratory chemicals, manufacture of substances.1.3 Details of the supplier of the safety data sheetCompany:MedChemExpress USATel:609-228-6898Fax:609-228-5909E-mail:sales@1.4 Emergency telephone numberEmergency Phone #:609-228-68982. HAZARDS IDENTIFICATION2.1 Classification of the substance or mixtureGHS Classification in accordance with 29 CFR 1910 (OSHA HCS)Acute toxicity, Oral (Category 4),H302Acute aquatic toxicity (Category 1),H400Chronic aquatic toxicity (Category 1),H4102.2 GHS Label elements, including precautionary statementsPictogramSignal word WarningHazard statement(s)H302 Harmful if swallowed.H410 Very toxic to aquatic life with long lasting effects.Precautionary statement(s)P264 Wash skin thoroughly after handling.P270 Do not eat, drink or smoke when using this product.P273 Avoid release to the environment.P301 + P312 IF SWALLOWED: Call a POISON CENTER or doctor/ physician if you feel unwell.P330 Rinse mouth.P391 Collect spillage.P501 Dispose of contents/ container to an approved waste disposal plant.2.3 Other hazardsNone.3. COMPOSITION/INFORMATION ON INGREDIENTS3.1 SubstancesSynonyms:SDZ⁻ASM 981Formula:C43H68ClNO11Molecular Weight:810.45CAS No. :137071-32-04. FIRST AID MEASURES4.1 Description of first aid measuresEye contactRemove any contact lenses, locate eye-wash station, and flush eyes immediately with large amounts of water. Separate eyelids with fingers to ensure adequate flushing. Promptly call a physician.Skin contactRinse skin thoroughly with large amounts of water. Remove contaminated clothing and shoes and call a physician.InhalationImmediately relocate self or casualty to fresh air. If breathing is difficult, give cardiopulmonary resuscitation (CPR). Avoid mouth-to-mouth resuscitation.IngestionWash out mouth with water; Do NOT induce vomiting; call a physician.4.2 Most important symptoms and effects, both acute and delayedThe most important known symptoms and effects are described in the labelling (see section 2.2).4.3 Indication of any immediate medical attention and special treatment neededTreat symptomatically.5. FIRE FIGHTING MEASURES5.1 Extinguishing mediaSuitable extinguishing mediaUse water spray, dry chemical, foam, and carbon dioxide fire extinguisher.5.2 Special hazards arising from the substance or mixtureDuring combustion, may emit irritant fumes.5.3 Advice for firefightersWear self-contained breathing apparatus and protective clothing.6. ACCIDENTAL RELEASE MEASURES6.1 Personal precautions, protective equipment and emergency proceduresUse full personal protective equipment. Avoid breathing vapors, mist, dust or gas. Ensure adequate ventilation. Evacuate personnel to safe areas.Refer to protective measures listed in sections 8.6.2 Environmental precautionsTry to prevent further leakage or spillage. Keep the product away from drains or water courses.6.3 Methods and materials for containment and cleaning upAbsorb solutions with finely-powdered liquid-binding material (diatomite, universal binders); Decontaminate surfaces and equipment by scrubbing with alcohol; Dispose of contaminated material according to Section 13.7. HANDLING AND STORAGE7.1 Precautions for safe handlingAvoid inhalation, contact with eyes and skin. Avoid dust and aerosol formation. Use only in areas with appropriate exhaust ventilation.7.2 Conditions for safe storage, including any incompatibilitiesKeep container tightly sealed in cool, well-ventilated area. Keep away from direct sunlight and sources of ignition.Recommended storage temperature:Powder-20°C 3 years4°C 2 yearsIn solvent-80°C 6 months-20°C 1 monthShipping at room temperature if less than 2 weeks.7.3 Specific end use(s)No data available.8. EXPOSURE CONTROLS/PERSONAL PROTECTION8.1 Control parametersComponents with workplace control parametersThis product contains no substances with occupational exposure limit values.8.2 Exposure controlsEngineering controlsEnsure adequate ventilation. Provide accessible safety shower and eye wash station.Personal protective equipmentEye protection Safety goggles with side-shields.Hand protection Protective gloves.Skin and body protection Impervious clothing.Respiratory protection Suitable respirator.Environmental exposure controls Keep the product away from drains, water courses or the soil. Cleanspillages in a safe way as soon as possible.9. PHYSICAL AND CHEMICAL PROPERTIES9.1 Information on basic physical and chemical propertiesAppearance White to off-white (Solid)Odor No data availableOdor threshold No data availablepH No data availableMelting/freezing point No data availableBoiling point/range No data availableFlash point No data availableEvaporation rate No data availableFlammability (solid, gas)No data availableUpper/lower flammability or explosive limits No data availableVapor pressure No data availableVapor density No data availableRelative density No data availableWater Solubility No data availablePartition coefficient No data availableAuto-ignition temperature No data availableDecomposition temperature No data availableViscosity No data availableExplosive properties No data availableOxidizing properties No data available9.2 Other safety informationNo data available.10. STABILITY AND REACTIVITY10.1 ReactivityNo data available.10.2 Chemical stabilityStable under recommended storage conditions.10.3 Possibility of hazardous reactionsNo data available.10.4 Conditions to avoidNo data available.10.5 Incompatible materialsStrong acids/alkalis, strong oxidising/reducing agents.10.6 Hazardous decomposition productsUnder fire conditions, may decompose and emit toxic fumes.Other decomposition products - no data available.11.TOXICOLOGICAL INFORMATION11.1 Information on toxicological effectsAcute toxicityClassified based on available data. For more details, see section 2Skin corrosion/irritationClassified based on available data. For more details, see section 2Serious eye damage/irritationClassified based on available data. For more details, see section 2Respiratory or skin sensitizationClassified based on available data. For more details, see section 2Germ cell mutagenicityClassified based on available data. For more details, see section 2CarcinogenicityIARC: No component of this product present at a level equal to or greater than 0.1% is identified as probable, possible or confirmed human carcinogen by IARC.ACGIH: No component of this product present at a level equal to or greater than 0.1% is identified as a potential or confirmed carcinogen by ACGIH.NTP: No component of this product present at a level equal to or greater than 0.1% is identified as a anticipated or confirmed carcinogen by NTP.OSHA: No component of this product present at a level equal to or greater than 0.1% is identified as a potential or confirmed carcinogen by OSHA.Reproductive toxicityClassified based on available data. For more details, see section 2Specific target organ toxicity - single exposureClassified based on available data. For more details, see section 2Specific target organ toxicity - repeated exposureClassified based on available data. For more details, see section 2Aspiration hazardClassified based on available data. For more details, see section 212. ECOLOGICAL INFORMATION12.1 ToxicityNo data available.12.2 Persistence and degradabilityNo data available.12.3 Bioaccumlative potentialNo data available.12.4 Mobility in soilNo data available.12.5 Results of PBT and vPvB assessmentPBT/vPvB assessment unavailable as chemical safety assessment not required or not conducted.12.6 Other adverse effectsNo data available.13. DISPOSAL CONSIDERATIONS13.1 Waste treatment methodsProductDispose substance in accordance with prevailing country, federal, state and local regulations.Contaminated packagingConduct recycling or disposal in accordance with prevailing country, federal, state and local regulations.14. TRANSPORT INFORMATIONDOT (US)This substance is considered to be non-hazardous for transport.IMDGUN number: 3077Class: 9Packing group: IIIEMS-No: F-A, S-FProper shipping name: ENVIRONMENTALLY HAZARDOUS SUBSTANCE, SOLID, N.O.S.Marine pollutant: Marine pollutant.IATAUN number: 3077Class: 9Packing group: IIIProper shipping name: Environmentally hazardous substance, solid, n.o.s.15. REGULATORY INFORMATIONSARA 302 Components:No chemicals in this material are subject to the reporting requirements of SARA Title III, Section 302.SARA 313 Components:This material does not contain any chemical components with known CAS numbers that exceed the threshold (De Minimis) reporting levels established by SARA Title III, Section 313.SARA 311/312 Hazards:No SARA Hazards.Massachusetts Right To Know Components:No components are subject to the Massachusetts Right to Know Act.Pennsylvania Right To Know Components:No components are subject to the Pennsylvania Right to Know Act.New Jersey Right To Know Components:No components are subject to the New Jersey Right to Know Act.California Prop. 65 Components:This product does not contain any chemicals known to State of California to cause cancer, birth defects, or anyother reproductive harm.16. OTHER INFORMATIONCopyright 2017 MedChemExpress. The above information is correct to the best of our present knowledge but does not purport to be all inclusive and should be used only as a guide. The product is for research use only and for experienced personnel. It must only be handled by suitably qualified experienced scientists in appropriately equipped and authorized facilities. The burden of safe use of this material rests entirely with the user. MedChemExpress disclaims all liability for any damage resulting from handling or from contact with this product.Caution: Product has not been fully validated for medical applications. For research use only.Tel: 609-228-6898 Fax: 609-228-5909 E-mail: tech@Address: 1 Deer Park Dr, Suite Q, Monmouth Junction, NJ 08852, USA。
美国Medchemexpress化合物库(小分子库)_Medchemexpress_(MCE中国)
美国Medchemexpress化合物库（小分子库）-原装进口，现货供
应，提供组合定制服务
品牌：Medchemexpress （MCE）
保存条件：-20℃
供应商：MCE中国
数量：大量
保质期：2年
Size：
Pre-dissolved DMSO/Solid（Or dry solid）
100 uL/well (10 mM solution)
200 uL/well (10 mM solution)
MedChemExpress (MCE)专注于各种抑制剂、调节剂、API、天然产物及化合物库，总部位于美国新泽西。
MCE经过十年努力已成为全球生物活性小分子领域的一流供应商。
MedChemExpress(MCE)产品涵盖近20个热门研究领域，1000多个细分靶点，超过3000个现货抑制剂、拮抗剂和激动剂。
相关的应用成果已发表于Nature、Cell等国际知名杂志，在全球20余个国家地区设有代理机构。
上海皓元生物医药科技有限公司(MCE 中国) 是MedChemExpress (MCE) 亚洲总代理。
MCE化合物库涵盖20余种不同的类型，超过2500个化合物，进口原装，
现货供应，提供详实的生物活性信息、化学结构信息、质控图谱（NMR和HPLC 等）。
还可根据您的实际研究需要，为您度身定制任意组合、规格、布板的特殊化合物库。
/screening-libraries.html
现有特色化合物库有：。
毛细管电泳-安培检测法测定夏枯草中的香豆素、芦丁与咖啡酸
毛细管电泳－安培检测法测定夏枯草中1的香豆素、芦丁与咖啡酸石焱芳、陈国南*教育部食品安全分析与检测技术重点实验室（福州大学），福州大学化学系，福州，福建，350002E-mail: gnchen@摘要：本章采用毛细管电泳安培检测法（CE-AD ），对香豆素、芦丁与咖啡酸三种中草药的有效成分进行分离分析。
在自组装仪器上，以0.5mm 碳圆盘微电极为工作电极，研究了电极电位，运行缓冲液浓度及酸度，分离电压和进样时间等因素对待测物的分离检测的影响，得到了最优化的分离条件。
在0.90V 的检测电位下，以50mmol/L 的硼酸－硼砂缓冲液（pH ＝8.95）为运行液，当毛细管长度为60cm ，分离电压为12kV 的时候，三组分在18min 内达到基线分离。
据此建立了香豆素、芦丁与咖啡酸三种化合物的毛细管电泳安培检测方法，并将该方法成功应用于夏枯草中三种物质含量的测定。
关键词：毛细管电泳安培检测法，香豆素，芦丁，咖啡酸1 引言夏枯草（学名为Prunella vulgaris Linn ，英文名为Common Selfheal ），为唇形科夏枯草属植物夏枯草的干燥果穗，因“此草夏至后即枯”得名[1]，是传统中药之一，一般取其干燥果实入药。
夏枯草属植物全球有15种，广泛分布于欧亚的温带地区、非洲西北部及北美洲，中国产4种及3个变种。
其味苦、性寒、辛，有清热明目、泻肝火、清热散结等功效。
其可用于治疗头痛眩晕，口眼歪斜，筋骨疼痛，目赤肿痛，畏光流泪，乳腺炎，乳癌，高血压（有降压、利尿作用），淋巴结核，浸润性肺结核，单纯性甲状腺肿，腮腺炎，急性黄疸型传染性肝炎，血崩，带下，猪、牛、羊传染性结膜炎、角膜炎等，对痢1本文得到教育部博士点基金（项目编号：20040386002）资助疾杆菌也有抑制作用[1-8]。
由于其重要的药用价值和广泛的药理作用，夏枯草越来越引起人们的关注。
多年来，国内外学者对夏枯草进行了广泛的研究，尤其是化学成分和药理作用面作了较为深入的探讨。
超高效液相色谱-串联质谱法测定化妆品中15种N-亚硝胺化合物
第42 卷第 11 期2023 年11 月Vol.42 No.111469~1478分析测试学报FENXI CESHI XUEBAO（Journal of Instrumental Analysis）超高效液相色谱-串联质谱法测定化妆品中15种N-亚硝胺化合物汪毅1，梁文耀1，何国山1，陈张好2，周智明2，吴谦1，席绍峰1，谭建华1*（1．广州质量监督检测研究院，国家化妆品质量检验检测中心（广州），广东广州511447；2．广东省药品检验所，广东广州510663）摘要：采用超高效液相色谱-串联质谱（UPLC-MS/MS）建立了化妆品中15种痕量N-亚硝胺化合物的分析方法。
水剂样品以水或乙腈分组超声提取，膏霜乳液样品采用亚铁氰化钾-乙酸锌溶液沉淀大分子或者饱和氯化钠-乙腈盐析分组处理后，以Agilent Poroshell 120 SB-Aq（100 mm×3.0 mm，2.7 μm）色谱柱分离，经大气压化学电离源（APCI）电离，多反应监测模式检测，以同位素内标法定量。
结果表明，15种N-亚硝胺化合物在相应质量浓度范围内线性关系良好（r2＞0.995），检出限和定量下限分别为5~15 ng/g和15~45 ng/g。
水、乳、膏霜3种化妆品基质在25、50、100 ng/g加标水平下的平均回收率为88.0%~111%，相对标准偏差（RSD，n=6）为1.4%~9.8%。
该方法用于市售化妆品检测，发现13批次样品检出N-亚硝基二乙醇胺（NDELA），其中1批次超限量值。
方法的专属性强，灵敏度高，精密度好，解决了N-亚硝胺化合物稳定性差、易被干扰等问题，适用于化妆品中15种N-亚硝胺化合物的痕量测定。
关键词：N-亚硝胺化合物；化妆品；超高效液相色谱-串联质谱法（UPLC-MS/MS）；大气压化学电离源中图分类号：O657.63；O623.732文献标识码：A 文章编号：1004-4957（2023）11-1469-10 Determination of Fifteen N-nitrosamine Compounds in Cosmetics by Ultra Performance Liquid Chromatography-TandemMass SpectrometryWANG Yi1，LIANG Wen-yao1，HE Guo-shan1，CHEN Zhang-hao2，ZHOU Zhi-ming2，WU Qian1，XI Shao-feng1，TAN Jian-hua1*（1．Guangzhou Quality Supervision and Testing Institute，National Quality Supervision and Testing Center for Cosmetics（Guangzhou），Guangzhou 511447，China；2．Guangdong Institute for Drug Control，Guangzhou 510663）Abstract：An ultra performance liquid chromatography-tandem mass spectrometric（UPLC-MS/MS）method was established for detecting 15 trace N-nitrosamine compounds in cosmetics. The final estab⁃lished method involved ultrasonic extraction of cosmetics using water or acetonitrile for different com⁃pounds. The samples were treated with potassium ferrocyanide-zinc acetate solution for precipitating macromolecules or saturated sodium chloride-acetonitrile for salting out.An Agilent Poroshell 120 SB-Aq（100 mm × 3.0 mm，2.7 μm） chromatography column was used for separation，followed by atmospheric pressure chemical ionization（APCI） source and multiple reaction monitoring mode detec⁃tion in the isotope internal standard method for quantification. The result showed good linearity（r2> 0.995） for the 15 N-nitrosamine compounds in their respective concentration ranges，with detection and quantitation limits of 5-15 ng/g and 15-45 ng/g，respectively.The average recoveries for the three cosmetic matrices（aqueous，emulsion，cream） at spiked levels of 25，50，100 ng/g were be⁃tween 88.0% and 111%，with relative standard deviations（RSD，n=6） of 1.4%-9.8%. The method was applied to the detection of commercial cosmetics and N-nitrosodiethanolamine（NDELA） was de⁃tected in 13 batches，with one batch exceeding the limit. The strong specificity，high sensitivity，and good precision made the method could solve the problems of poor stability and easy interference ofdoi：10.19969/j.fxcsxb.23051602收稿日期：2023－05－16；修回日期：2023－06－10基金项目：广东省药品监督管理局化妆品风险评估重点实验室专项（2021ZDZ03）；广东省市场监督管理局科技项目（2022CZ06）∗通讯作者：谭建华，博士，正高级工程师，研究方向：色谱－质谱检测技术研究，E-mail：tanjianhua0734@第 42 卷分析测试学报N-nitrosamine compounds，and was suitable for the trace determination of 15 N-nitrosamine com⁃pounds in cosmetics.Key words：N-nitrosamine compounds；cosmetics；ultra performance liquid chromatography-tan⁃dem mass spectrometry（UPLC-MS/MS）；atmospheric pressure chemical ionization（APCI） sourceN-亚硝胺化合物是一类具有N-亚硝基结构的化合物，因取代基的不同，形成了种类繁多的同系物，目前已发现超过300种［1］。
不同部位脑梗死华勒变性的特点及对神经功能的影响
［8］涂梦恬，李良平.肝细胞核因子受体4α在非酒精性脂肪性肝病中的研究现状［J］.国际消化病杂志，2017，37（3）：144-147.Tu MT，Li LP.Research status of hepatocyte nuclear factor receptor4αin nonalcoholic fatty liver disease［J］.Int J Gastroenterol，2017，37（3）：144-147.doi：10.3969/j.issn.1673-534X.2017.03.003.［9］Thayer TE，Lino Cardenas CL，Martyn T，et al.The role of bone morphogenetic protein signaling in non-alcoholic fatty liver disease ［J］.Sci Rep，2020，10（1）：9831.doi：10.1038/s41598-020-66770-8.［10］Cariou B，Byrne CD，Loomba R，et al.NAFLD as a metabolic disease in humans：A literature review［J］.Diabetes Obes Metab，2021，23（5）：1069-1083.doi：10.1111/dom.14322.［11］Theofilatos D，Anestis A，Hashimoto K，et al.Transcriptional regulation of the human liver X receptorαgene by hepatocyte nuclear factor4α［J］.Biochem Biophys Res Commun，2016，469（3）：573-579.doi：10.1016/j.bbrc.2015.12.031.［12］Vespasiani-Gentilucci U，Dell'Unto C，De Vincentis A，et al. Combining genetic variants to improve risk prediction for NAFLD and its progression to cirrhosis：a proof of concept study［J］.Can J Gastroenterol Hepatol，2018，2018：7564835.doi：10.1155/2018/ 7564835.［13］Khalid YS，Dasu NR，Suga H，et al.Increased cardiovascular events and mortality in females with NAFLD：a meta-analysis［J］. Am J Cardiovasc Dis，2020，10（3）：258-271.［14］Trépo E，Valenti L.Update on NAFLD genetics：From new variants to the clinic［J］.J Hepatol，2020，72（6）：1196-1209.doi：10.1016/ j.jhep.2020.02.020.［15］Matsuo S，Ogawa M，Muckenthaler MU，et al.Hepatocyte nuclear factor4alpha controls iron metabolism and regulates transferrin receptor2in mouse liver［J］.J Biol Chem，2015，290（52）：30855-30865.doi：10.1074/jbc.M115.694414.［16］Chi X，Wei X，Gao W，et al.Dexmedetomidine ameliorates acute lung injury following orthotopic autologous liver transplantation in rats probably by inhibiting Toll-like receptor4-nuclear factor kappa B signaling［J］.J Transl Med，2015，13：190.doi：10.1186/ s12967-015-0554-5.［17］Wang L，Yao M，Zheng W，et al.Insulin-like growth factor I receptor：a novel target for hepatocellular carcinoma gene therapy ［J］.Mini Rev Med Chem，2019，19（4）：272-280.doi：10.2174/ 1389557518666181025151608.（2020-10-23收稿2021-01-17修回）（本文编辑李鹏）不同部位脑梗死华勒变性的特点及对神经功能的影响王冬梅，蔡桂淑，刘立生△摘要：目的探讨不同部位脑梗死华勒变性的特点及对神经功能的影响。
高效液相色谱质谱法测定食品接触材料着色剂中芳香胺类物质
高效液相色谱质谱法测定食品接触材料着色剂中芳香胺类物质花 锦1*，肖利龙2（1.太原海关技术中心，山西太原 030001；2.太原学院，山西太原 030001）摘 要：目的：建立高效液相色谱质谱法测定食品接触材料中着色剂中芳香胺类物质。
方法：用乙腈超声提取试样中芳香胺类物资，改进QuEChERS 法净化，使用ACQUITY HSS T3柱以水和甲醇溶液进行梯度洗脱，采用电离喷雾电离方式（ESI+），通过多反应监测（MRM）定量。
结果：该法测定时间短，在5 min 内出峰，线性关系良好，相关系数r 大于0.99，回收率在67.0%～95.0%，相对标准偏差（RSD ）均小于15%。
该法快速、简便、精确度高、准确度高，对食品级着色剂中芳香胺残留有普遍适用性，其他着色剂可参考使用。
关键词：QuEChERS；食品接触材料；芳香胺；着色剂；液相色谱质谱联用食品接触材料通常是指与食物直接接触的物质，在带来生活上便利的同时也带来了食品安全问题。
着色剂是指能给予或改变食品包装材料颜色的物质，通常包括染料和颜料两种，此外还有一些特殊物质如光学增量剂、荧光漂白剂等本身没有颜色但能提高产品光亮的物质，主要用于提高产品的美观。
因此食品接触材料中会存在着色剂，其中偶氮类染料最为常见。
偶氮染料具有色谱范围广，牢度强，着色快，色光好等优势，因此偶氮染料的使用较为广泛，不仅应用于食品接触材料，还应用于皮革、纺织、化妆品、纸张等生活必需品[1]。
早在20世纪，有日本人发现偶氮染料中的溶剂黄可导致老鼠的肝细胞发生癌变，之后1905年德国也从染料品红、萘胺等物质中发现了偶氮染料的致癌性[2]。
偶氮染料主要通过分解为芳香胺来释放有毒有害物质，分解过程见 图1。
图1 芳香族偶氮染料分解为芳香胺芳香胺类物质对人类健康和环境具有危害性，尤其是2,4-二甲基苯胺、2-萘胺、对氯苯胺等，进入人体之后会产生高铁血红蛋白引起一系列疾病[3]。
由于食品安全方面芳香胺的危害较大，而我国目前对于食品接触材料中芳香胺的检测技术还不够全面，只对接触材料进行了研究，对其中着色剂没有深入探讨，因此芳香胺的检测方案急需优化以及扩充。
《国际药学研究杂志》稿约
《国际药学研究杂志》原名《国外医学药学分册》，是军事医学科学院主管、军事医学科学院毒物药物研究所和中国药学会主办的大型综合性药学刊物，为月刊，国内外公开发行。
设置有专家论坛、专题报道、综述、论著、医药信息等栏目。
本刊以从事药学研究的科技人员、临床医师和药师、制药工程技术人员、医药院校师生为读者对象，根据国内药学科研、教学、临床和生产的需要，追踪报道国际药学领域的新进展、新动向、新技术和新成果，包括药物化学、药剂学、药物代谢、药物分析、药理和毒理学、生化药学和临床药学等基础研究和应用研究方面的内容。
是中国科技论文统计源期刊（中国科技核心期刊）、北大图书馆中文核心期刊，中国生物医学核心期刊，被美国《化学文摘》、美国《剑桥科学文摘》、荷兰《医学文摘》、世界卫生组织西太平洋地区医学索引、英国《农业与生物科学研究中心数据库》、中国核心期刊（遴选）数据库、中文科技期刊数据库、中国学术期刊综合评价数据库、中国生物医学期刊引文数据库、中文生物医学期刊文献数据库、中国药学文献数据库和中国生物学文献数据库等多个国内外权威检索系统收录。
2011、2014年连续两届被评为“中国精品科技期刊”。
多篇论文入选“F5000中国精品科技期刊顶尖学术论文”及中国药学会优秀论文。
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欧当归内酯A对实验性纤维化肝脏NO及内皮细胞功能的影响
欧当归内酯A对实验性纤维化肝脏NO及内皮细胞功能的影响作者：赵志敏黄恺沈丽刘成海叶伟成来源：《世界中医药》2020年第19期摘要目的：探讨欧当归内酯A调节纤维化肝脏NO释放的抗肝纤维化作用机制。
方法：40只Wistar大鼠随机分为正常组、模型组、欧当归内酯A 3 mg/kg组、欧当归内酯A 6 mg/kg 组，每组10只。
以四氯化碳（CCl4）与高脂低蛋白饮食复合因素诱导肝纤维化模型，连续6周。
药物观察组于造模第4周腹腔注射给药至结束。
观察肝组织炎性反应及胶原沉积、eNOS 表达及MDA、SOD、NO、NOS水平。
体外以800 μmol/L氯化钴作用于SK-HEP-1细胞24 h 诱导细胞缺氧损伤，药物处理后观察细胞活力、vWF表达、上清及胞内NO水平。
结果：与模型组比较，欧当归内酯A各组肝细胞变性和炎性反应坏死有所减轻，纤维化改善;高剂量组SOD和MDA显著改善，NO和NOS降低，eNOS阳性表达下降（P<0.05）。
体外实验显示，药物干预后细胞活力得到改善，vWF平均荧光强度减弱，NO释放显著改善（P<0.05）。
结论：欧当归内酯A具有抗肝纤维化的作用，其机制可能与抗脂质过氧化损伤，改善内皮细胞功能，调节NO释放有关。
关键词肝纤维化;欧当归内酯A;内皮细胞;一氧化氮;机制AbstractObjective：To explore the effects of levistilide A on anti-hepatic fibrosis mechanism of regulating the release of NO from fibrotic liver. Methods：A total of 40 Wistar rats were randomly divided a control group， a model group， a levistilide A 3 mg/kg group and a levistilide 6 mg/kg group， with 10 rats in each group. The liver fibrosis model was induced by a combination of carbon tetrachloride （CCl4） and a high-fat and low-protein diet for 6 consecutive weeks. The drug treatment group was given intraperitoneal injection to the end on the 4th week of modeling. Liver tissue inflammatory reaction and collagen deposition， eNOS expression and MDA， SOD， NO，NOS levels were observed. In vitro，800 μmol/L cobalt chloride was applied to SK-HEP-1 cells for 24 h to induce cell hypoxia. After drug treatment， cell viability， vWF expression， supernatant and intracellular NO levels were observed. Results：Compared with those in the model group， the degeneration and inflammatory necrosis of Levistilide A in each group were reduced， and the fibrosis was improved; the high-dose group SOD and MDA significantly improved， NO and NOS decreased， and the positive expression of eNOS decreased （P<0.05）. In vitro experiments showed that cell viability was improved after drug intervention， the average fluorescence intensity of vWFwas weakened， and the release of NO was significantly improved （P<0.05）. Conclusion：Levistilide A can inhibit liver fibrosis， the mechanism may be related to Levistilide A， anti-lipid peroxidation， and regulate the release of NO.KeywordsLiver fibrosis; Levistilide A; Endothelial cell; Nitric oxide; Mechanism 中圖分类号：R285.5文献标识码：Adoi：10.3969/j.issn.1673-7202.2020.19.004肝纤维化存在于大多数慢性肝脏疾病过程中，肝组织内细胞外基质过度增生与沉积导致肝脏组织结构异常改变，并影响肝脏正常生理功能，是慢性肝病过程中一种可逆的肝组织损伤过度修复反应[1]。
超高效液相色谱-串联质谱法测定全麦粉中的赭曲霉毒素A
超高效液相色谱-串联质谱法测定全麦粉中的赭曲霉毒素A唐德红，张 季，张冰雪，任 伟，张丹丹，刘 冲*（遵义市产品质量检验检测院，贵州遵义 563000）摘 要：目的：建立超高效液相色谱-串联质谱法测定全麦粉中赭曲霉毒素A的含量。
方法：全麦粉样品经甲醇-水（60∶40，V∶V）提取，磷酸盐缓冲溶液稀释，赭曲霉毒素A免疫亲和柱净化，超高效液相色谱-串联质谱测定分析，内标法定量。
结果：赭曲霉毒素A在0.475～9.500 ng·mL-1具有良好的线性关系（R2=0.999 9），3个加标水平下的平均回收率为85.62%～99.42%，相对标准偏差为1.92%～4.66%，检出限为0.68 μg·kg-1、定量限为2.27 μg·kg-1。
结论：该方法便捷、稳定、灵敏度高、准确度好，可用于快速分析全麦粉中赭曲霉毒素A的含量。
关键词：全麦粉；赭曲霉毒素A；超高效液相色谱-串联质谱Determination of Ochratoxin A in Whole Wheat Flour by Ultra Performance Liquid Chromatography-Tandem MassSpectrometryTANG Dehong, ZHANG Ji, ZHANG Bingxue, REN Wei, ZHANG Dandan, LIU Chong*(Product Quality Inspection and Testing Institute in Zunyi, Zunyi 563000, China) Abstract: Objective: To establish an ultra high performance liquid chromatography-tandem mass spectrometry method for the determination of ochratoxin A in whole wheat flour. Method: Whole wheat flour samples were extracted with methanol water (60∶40, V∶V), diluted with phosphate buffer solution, purified with ochratoxin A immunoaffinity column, analyzed by ultra-high performance liquid chromatography tandem mass spectrometry, and quantified by internal standard method. Result: Ochratoxin A ranges from 0.475 ng·mL-1 to 9.500 ng·mL-1 has a good linear relationship (R2=0.999 9). The recovery rates at three spiked levels were 85.62%～99.42%,the relative standard deviation was 1.92%～4.66%, and the detection limit was 0.68 μg·kg-1, with a quantification limit of 2.27 μg·kg-1. Conclusion: This method is convenient, stable, sensitive, and accurate, and can be used for rapid analysis of ochratoxin A content in whole wheat flour.Keywords: whole wheat flour; ochratoxin A; ultra performance liquid chromatography-tandem mass spectrometry赭曲霉毒素A（Ochratoxin A，OTA）是食物中最常见的霉菌毒素之一[1]，是曲霉属和青霉属的真菌形成的次级代谢产物[2-4]，广泛存在于各种食物中。
高效液相色谱内标法检测鸡血浆中甲砜霉素的浓度
高效液相色谱内标法检测鸡血浆中甲砜霉素的浓度张小华;陶冠红;陈园;陈晓兰;王妲妲【期刊名称】《化学分析计量》【年(卷),期】2010(019)002【摘要】以氟甲砜霉素作内标,乙腈作为提取溶剂,采用高效液相色谱内标法检测鸡血浆中甲砜霉素的浓度.色谱柱为Shim-pack CLC-ODS(150 mm×6 mm,5μm),流动相为乙腈-水(体积比25:75),流速为1.0 mL/min,检测波长为225 nm,柱温为40℃.在此色谱条件下,在0.25～32.00 mG/L浓度范围内,甲砜霉素浓度与甲砜霉素和氟甲砜霉素峰面积比呈线性关系,相关系数r为0.9999,最低检测浓度为0.1mg/L;在高、中、低3个浓度水平下日内、日间精密度均大于6.1%(n=5),提取回收率大于98.68%,方法回收率为99.20%～100.25%.建立的方法符合生物样品的分析要求,可用于临床药代动力学研究.【总页数】4页(P48-51)【作者】张小华;陶冠红;陈园;陈晓兰;王妲妲【作者单位】江苏畜牧兽医职业技术学院药物检测中心,泰州,225300;苏州大学化学化工学院,苏州,215123;苏州大学化学化工学院,苏州,215123;江苏畜牧兽医职业技术学院药物检测中心,泰州,225300;江苏畜牧兽医职业技术学院药物检测中心,泰州,225300;江苏畜牧兽医职业技术学院药物检测中心,泰州,225300【正文语种】中文【相关文献】1.高效液相色谱法同时检测水产品中氯霉素、甲砜霉素与氟甲砜霉素残留 [J], 杨方;陈国南2.超高效液相色谱-串联质谱法同时检测人血浆中11种镇静催眠药浓度∗ [J], 安静;董占军;魏欣;白万军;宋浩静3.高效液相色谱荧光检测法检测鸡肉中甲砜霉素残留 [J], 谢恺舟;徐东;陈书琴;谢星;黄玉萍;贾龙飞;郭辉生;王金玉4.水产品中氯霉素、甲砜霉素和氟甲砜霉素残留量高效液相色谱-串联质谱内标测定方法的研究 [J], 王志杰;冷凯良;孙伟红;刘艳萍;翟毓秀;谭志军;郭萌萌;王瑜5.同时测定人血浆中甲砜霉素和前药甲砜霉素甘氨酸酯浓度及其药代动力学研究[J], 闫合峰;周成林;韩德恩因版权原因，仅展示原文概要，查看原文内容请购买。
液相色谱_质谱联用法检测非法制剂中的醋酸泼尼松
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线性关系考察： 精密吸取甲氧 苄啶对照品溶液 （ &- &$" :& +> 5 +6） 注入液相色 %， 9- % ， 2& ， 2!- % ， 2% !6， 谱仪， 按拟订的色谱条件依法测定， 记录色谱图。 以进样量为横坐标、 峰 面积积分值为纵坐标进行线性回归， 计算得回归方程 & ? %79 777- 2 ’ J 。 结果 ! ? &- """ " （ " ? .） 2 2&:- ."! ， 表 明 甲 氧 苄 啶 进 样 量 在 &- !$" = &- 9$9 !> 范围内与峰面积积分值线 性关系良好。 精密度试验： 精密吸取甲氧苄啶 对照品溶液（ &- &$" :& +> 5 +6） 2& !6， 注入液相色谱仪， 重复进样 . 次， 依 法测 定。 结 果 峰面 积 积 分平 均 值为 ， 表明 !.9 &:. ，#$% ? 2- !@ （ " ? .） 仪器精密度良好。 取同一批 （ 批号为 样品I 分为两组， 由不同 !&&.&%2! ） 操作人员在不同设备上进行含量测定。 结果两组含量平均值为标 ， 表明方法中间精密度良好。 示量的 ":- 9@ ， #$% ? &- .&@ （ " ? .） 稳定性试验： 精密吸取同一供试品溶液（ 批 号 为 !&&.&%2! ） 注入液相色谱仪， 每 ! K 进样 2 次， 测定 % 次。 结果甲氧苄啶 2& !6， ， 表明供试品 峰面积积分平均值为 !.. 92" ， #$% ? &- !!@ （ " ? .） 溶液在 : K 内基本稳定。 加样回收试验 L 取已知含量的样品 （ 批号为 !&&.&%2! ） 细粉， 按
液相色谱-质谱联用技术测定头孢他啶中未知杂质的结构
液相色谱-质谱联用技术测定头孢他啶中未知杂质的结构欧贝丽;曲斌;陈德英;胡育筑
【期刊名称】《海峡药学》
【年(卷),期】2008(020)003
【摘要】目的应用液相色谱-电喷雾离子化质谱法分析头孢他啶原料药中的杂质,并初步确定了一未知杂质的结构.方法采用C18色谱柱;以乙腈-乙酸铵水溶液(15:85)为流动相;检测波长255nm;以电喷雾电离源正离子模式进行质谱数据采集.结果获得头孢他啶和未知杂质的液相色谱图以及液相色谱峰对应的一级质谱图,对谱图进行分析归纳,推测头孢他啶样品中未知杂质的结构为头孢他啶结构中羧酸的甲酯化产物.结论本方法灵敏、可靠、快速,对头孢他啶的生产、质量监控具有指导意义.
【总页数】3页(P48-50)
【作者】欧贝丽;曲斌;陈德英;胡育筑
【作者单位】中国药科大学分析化学教研室,南京,210009;中国药科大学分析化学教研室,南京,210009;中国药科大学分析化学教研室,南京,210009;中国药科大学分析化学教研室,南京,210009
【正文语种】中文
【中图分类】R927
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2.液相色谱-质谱/质谱联用技术在测定白酒中甜蜜素含量中的应用 [J], 陈海元;王永健;
3.二维超高效液相色谱质谱联用技术测定注射用头孢地嗪钠的杂质谱 [J], 杨倩;伏圣青;王静
4.二维超高效液相色谱-飞行时间质谱联用技术鉴定氯化琥珀胆碱原料药中的杂质[J], 陈红;杨梅;张姮婕;袁铭;廉向金
5.高效液相色谱/质谱联用技术快速鉴定左氧氟羧酸原料药中微量未知杂质 [J],因版权原因，仅展示原文概要，查看原文内容请购买。