NS-398_LCMS_19277_MedChemExpress

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NS-398_SDS_MedChemExpress

NS-398_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 :NS-398Catalog No. :HY-13913CAS No. :123653-11-21.2 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:NS 398; NS398Formula:C13H18N2O5SMolecular Weight:314.36CAS No. :123653-11-24. 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 Light yellow to yellow (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.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 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。

S1771 NS-398_COX-2抑制剂_

S1771 NS-398_COX-2抑制剂_

NS-398 (COX-2抑制剂)
产品编号产品名称包装
(COX-2抑制剂) 1mg S1771 NS-398
产品简介:
¾NS-398,是一种选择性环氧合酶-2(cyclooxygenase-2, COX-2, 即PGH synthase-2)的抑制剂。

NS-398对于人COX-2的IC50根据不同的文献约为0.1-1.77µM,而对于人COX-1的IC50根据不同文献仅约为75-100µM。

因此NS-398是一种COX-2选择性抑制剂。

¾NS-398可以穿透细胞膜,可以用于特异性地抑制细胞内的COX-2。

本产品可以用于培养细胞,也可以用于动物实验。

¾NS-398分子量为314.36,分子式为C13H18N2O5S,CAS Number:123653-11-2。

本产品为进口分装,纯度大于98%。

¾NS-398不溶于水,可溶于DMSO或二甲基酰胺,在适当温育或超声处理条件下可以溶解于无水乙醇。

¾本NS-398用DMSO配制,浓度为10mg/ml,共0.1ml。

包装清单:
产品编号产品名称包装
(COX-2抑制剂, 10mg/ml) 1mg
S1771 NS-398
— 说明书1份
保存条件:
-20℃保存。

注意事项:
¾为了您的安全和健康,请穿实验服并戴一次性手套操作。

使用说明:
1. NS-398常见使用浓度为10µM。

具体的最佳工作浓度请参考相关文献,或根据实验目的,以及所培养的特定细胞和组织,
通过实验进行摸索和优化。

Gelucire-14-44-SDS-MedChemExpress

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。

marked manuscript

marked manuscript

Quality evaluation of Flos Lonicerae through a simultaneous determination of seven saponins by HPLC with ELSDXing-Yun Chai1, Song-Lin Li2, Ping Li1*1Key Laboratory of Modern Chinese Medicines and Department of Pharmacognosy, China Pharmaceutical University, Nanjing, 210009, People’s Republic of China2Institute of Nanjing Military Command for Drug Control, Nanjing, 210002, People’s Republic of China*Corresponding author: Ping LiKey Laboratory of Modern Chinese Medicines and Department of Pharmacognosy, China Pharmaceutical University, Nanjing 210009, People’s Republic of China.E-mail address: lipingli@Tel.: +86-25-8324-2299; 8539-1244; 135********Fax: +86-25-8532-2747AbstractA new HPLC coupled with evaporative light scattering detection (ELSD) method has been developed for the simultaneous quantitative determination of seven major saponins, namely macranthoidinB (1), macranthoidin A (2), dipsacoside B (3), hederagenin-28-O-β-D-glucopyranosyl(6→1)-O-β-D- glucopyranosyl ester (4), macranthoside B (5), macranthoside A (6), and hederagenin-3-O-α-L-arabinopyranosyl(2→1)-O-α-L-rhamnopyranoside (7)in Flos Lonicerae, a commonly used traditional Chinese medicine (TCM) herb.Simultaneous separation of these seven saponins was achieved on a C18 analytical column with a mixed mobile phase consisting of acetonitrile(A)-water(B)(29:71 v/v) acidified with 0.5% acetic acid. The elution was operated from keeping 29%A for 10min, then gradually to 54%B from 10 to 25 min on linear gradient, and then keep isocratic elution with 54%B from 25 to 30min.The drift tube temperature of ELSD was set at 106℃, and with the nitrogen flow-rate of 2.6 l/min. All calibration curves showed good linear regression (r2 0.9922) within test ranges. This method showed good reproducibility for the quantification of these seven saponins in Flos Lonicerae with intra- and inter-day variations of less than 3.0% and 6.0% respectively. The validated method was successfully applied to quantify seven saponins in five sources of Flos Lonicerae, which provides a new basis of overall assessment on quality of Flos Lonicerae.Keywords: HPLC-ELSD; Flos Lonicerae; Saponins; Quantification1. IntroductionFlos Lonicerae (Jinyinhua in Chinese), the dried buds of several species of the genus Lonicera (Caprifoliaceae), is a commonly used traditional Chinese medicine (TCM) herb. It has been used for centuries in TCM practice for the treatment of sores, carbuncles, furuncles, swelling and affections caused by exopathogenic wind-heat or epidemic febrile diseases at the early stage [1]. Though four species of Lonicera are documented as the sources of Flos Lonicerae in China Pharmacopeia (2000 edition), i.e. L. japonica, L. hypoglauca,L. daystyla and L. confusa, other species such as L. similes and L. macranthoides have also been used on the same purpose in some local areas in China [2]. So it is an important issue to comprehensively evaluate the different sources of Flos Lonicerae, so as to ensure the clinical efficacy of this Chinese herbal drug.Chemical and pharmacological investigations on Flos Lonicerae resulted in discovering several kinds of bioactive components, i.e. chlorogenic acid and its analogues, flavonoids, iridoid glucosides and triterpenoid saponins [3]. Previously, chlorogenic acid has been used as the chemical marker for the quality evaluation of Flos Lonicerae,owing to its antipyretic and antibiotic property as well as its high content in the herb. But this compound is not a characteristic component of Flos Lonicerae, as it has also been used as the chemical marker for other Chinese herbal drugs such as Flos Chrysanthemi and so on[4-5]. Moreover, chlorogenic acid alone could not be responsible for the overall pharmacological activities of Flos Lonicerae[6].On the other hand, many studies revealed that triterpenoidal saponins of Flos Lonicerae possess protection effects on hepatic injury caused by Acetaminophen, Cd, and CCl4, and conspicuous depressant effects on swelling of ear croton oil [7-11]. Therefore, saponins should also be considered as one of the markers for quality control of Flos Lonicerae. Consequently, determinations of all types of components such as chlorogenic acid, flavonoids, iridoid glucosides and triterpenoidal saponins in Flos Lonicerae could be a better strategy for the comprehensive quality evaluation of Flos Lonicerae.Recently an HPLC-ELSD method has been established in our laboratory for qualitative and quantitative determination of iridoid glucosides in Flos Lonicerae [12]. But no method was reported for the determination of triterpenoidal saponins in Flos Lonicera. As a series studies on the comprehensive evaluation of Flos Lonicera, we report here, for the first time, the development of an HPLC-ELSD method for simultaneous determination of seven triterpenoidal saponins in the Chinese herbal drug Flos Lonicerae, i.e.macranthoidin B (1), macranthoidin A (2), dipsacoside B (3), hederagenin-28-O-β-D-glucopyranosyl(6→1)-O-β-D- glucopyranosyl ester (4), macranthoside B (5), macranthoside A (6), and hederagenin-3-O-α-L-arabinopyranosyl(2→1)-O-α-L-rhamnopyranoside (7) (Fig. 1).2. Experimental2.1. Samples, chemicals and reagentsFive samples of Lonicera species,L. japonica from Mi county, HeNan province (LJ1999-07), L. hypoglauca from Jiujang county, JiangXi province (LH2001-06), L. similes from Fei county, ShanDong province (LS2001-07), L. confuse from Xupu county, HuNan province (LC2001-07), and L. macranthoides from Longhu county, HuNan province (LM2000-06) respectively, were collected in China. All samples were authenticated by Dr. Ping Li, professor of department of Pharmacognosy, China Pharmaceutical University, Nanjing, China. The voucher specimens were deposited in the department of Pharmacognosy, China Pharmaceutical University, Nanjing, China. Seven saponin reference compounds: macranthoidin B (1), macranthoidin A (2), dipsacoside B (3), hederagenin-28-O-β-D-glucopyranosyl(6→1)-O-β-D- glucopyranosyl ester (4), macranthoside B (5), macranthoside A (6), and hederagenin-3-O-α-L-arabinopyranosyl(2→1)-O-α-L-rhamnopyranoside (7) were isolated previously from the dried buds of L. confusa by repeated silica gel, sephadex LH-20 and Rp-18 silica gel column chromatography, their structures were elucidated by comparison of their spectral data (UV, IR, MS, 1H- NMR and 13C-NMR) with references [13-15]. The purity of these saponins were determined to be more than 98% by normalization of the peak areas detected by HPLC with ELSD, and showed very stable in methanol solution.HPLC-grade acetonitrile from Merck (Darmstadt, Germany), the deionized water from Robust (Guangzhou, China), were purchased. The other solvents, purchased from Nanjing Chemical Factory (Nanjing, China) were of analytical grade.2.2. Apparatus and chromatographic conditionsAglient1100 series HPLC apparatus was used. Chromatography was carried out on an Aglient Zorbax SB-C18 column(250 4.6mm, 5.0µm)at a column temperature of 25℃.A Rheodyne 7125i sampling valve (Cotati, USA) equipped with a sample loop of 20µl was used for sample injection. The analog signal from Alltech ELSD 2000 (Alltech, Deerfield, IL, USA)was transmitted to a HP Chemstation for processing through an Agilent 35900E (Agilent Technologies, USA).The optimum resolution was obtained by using a linear gradient elution. The mobile phase was composed of acetonitrile(A) and water(B) which acidified with 0.5% acetic acid. The elution was operated from keeping 29%A for 10min, then gradually to 54%B from 10 to 25 min in linear gradient, and back to the isocratic elution of 54%B from 25 to 30 min.The drift tube temperature for ELSD was set at 106℃and the nitrogen flow-rate was of 2.6 l/min. The chromatographic peaks were identified by comparing their retention time with that of each reference compound tried under the same chromatographic conditions with a series of mobile phases. In addition, spiking samples with the reference compounds further confirmed the identities of the peaks.2.3. Calibration curvesMethanol stock solutions containing seven analytes were prepared and diluted to appropriate concentration for the construction of calibration curves. Six concentrationof the seven analytes’ solution were injected in triplicate, and then the calibration curves were constructed by plotting the peak areas versus the concentration of each analyte. The results were demonstrated in Table1.2.4. Limits of detection and quantificationMethanol stock solution containing seven reference compounds were diluted to a series of appropriate concentrations with methanol, and an aliquot of the diluted solutions were injected into HPLC for analysis.The limits of detection (LOD) and quantification (LOQ) under the present chromatographic conditions were determined at a signal-to-noise ratio (S/N) of 3 and 10, respectively. LOD and LOQ for each compound were shown in Table1.2.5. Precision and accuracyIntra- and inter-day variations were chosen to determine the precision of the developed assay. Approximate 2.0g of the pulverized samples of L. macranthoides were weighted, extracted and analyzed as described in 2.6 Sample preparation section. For intra-day variability test, the samples were analyzed in triplicate for three times within one day, while for inter-day variability test, the samples were examined in triplicate for consecutive three days. Variations were expressed by the relative standard deviations. The results were given in Table 2.Recovery test was used to evaluate the accuracy of this method. Accurate amounts of seven saponins were added to approximate 1.0g of L. macranthoides,and then extracted and analyzed as described in 2.6 Sample preparation section. The average recoveries were counted by the formula: recovery (%) = (amount found –original amount)/ amount spiked ×100%, and RSD (%) = (SD/mean) ×100%. The results were given in Table 3.2.6. Sample preparationSamples of Flos Lonicerae were dried at 50℃until constant weight. Approximate 2.0g of the pulverized samples, accurately weighed, was extracted with 60% ethanol in a flask for 4h. The ethanol was evaporated to dryness with a rotary evaporator. Residue was dissolved in water, followed by defatting with 60ml of petroleum ether for 2 times, and then the water solution was evaporated, residue was dissolved with methanol into a 25ml flask. One ml of the methanol solution was drawn and transferred to a 5ml flask, diluted to the mark with methanol. The resultant solution was at last filtrated through a 0.45µm syringe filter (Type Millex-HA, Millipore, USA) and 20µl of the filtrate was injected to HPLC system. The contents of the analytes were determined from the corresponding calibration curves.3. Results and discussionsThe temperature of drift tube and the gas flow-rate are two most important adjustable parameters for ELSD, they play a prominent role to an analyte response. In ourprevious work [12], the temperature of drift tube was optimized at 90°C for the determination of iridoids. As the polarity of saponins are higher than that of iridoids, more water was used in the mobile phase for the separation of saponins, therefore the temperature for saponins determination was optimized systematically from 95°C to 110°C, the flow-rate from 2.2 to 3.0 l/min. Dipsacoside B was selected as the testing saponin for optimizing ELSD conditions, as it was contained in all samples. Eventually, the drift tube temperature of 106℃and a gas flow of 2.6 l/min were optimized to detect the analytes. And these two exact experimental parameters should be strictly controlled in the analytical procedure [16].All calibration curves showed good linear regression (r2 0.9922) within test ranges. Validation studies of this method proved that this assay has good reproducibility. As shown in Table 2, the overall intra- and inter-day variations are less than 6% for all seven analytes. As demonstrated in Table 3, the developed analytical method has good accuracy with the overall recovery of high than 96% for the analytes concerned. The limit of detection (S/N=3) and the limit of quantification (S/N=10) are less than 0.26μg and 0.88μg respectively (Table1), indicating that this HPLC-ELSD method is precise, accurate and se nsitive enough for the quantitative evaluation of major non- chromaphoric saponins in Flos Lonicerae.It has been reported that there are two major types of saponins in Flos Lonicerae, i.e. saponins with hederagenin as aglycone and saponins with oleanolic acid as the aglycone [17]. But hederagenin type saponins of the herb were reported to have distinct activities of liver protection and anti-inflammatory [7-11]. So we adoptedseven hederagenin type saponins as representative markers to establish a quality control method.The newly established HPLC-ELSD method was applied to analyze seven analytes in five plant sources of Flos Lonicerae, i.e. L. japonica,L. hypoglauca,L. confusa,L. similes and L. macranthoides(Table 4). It was found that there were remarkable differences of seven saponins contents between different plant sources of Flos Lonicerae. All seven saponins analyzed could be detected in L. confusa and L. hypoglauca, while only dipsacoside B was detected in L. japonica. Among all seven saponins interested, only dipsacoside B was found in all five plant species of Flos Lonicerae analyzed, and this compound was determined as the major saponin with content of 53.7 mg/g in L. hypoglauca. On the other hand, macranthoidin B was found to be the major saponin with the content higher than 41.0mg/g in L. macranthoides,L. confusa, and L. similis, while the contents of other analytes were much lower.In our previous study [12], overall HPLC profiles of iridoid glucosides was used to qualitatively and quantitatively distinguish different origins of Flos Lonicerae. As shown in Fig.2, the chromatogram profiles of L. confusa, L. japonica and L. similes seem to be similar, resulting in the difficulty of clarifying the origins of Flos Lonicerae solely by HPLC profiles of saponins, in addition to the clear difference of the HPLC profiles of saponins from L. macranthoides and L. hypoglauca.Therefore, in addition to the conventional morphological and histological identification methods, the contents and the HPLC profiles of saponins and iridoids could also be used as accessory chemical evidence toclarify the botanical origin and comprehensive quality evaluation of Flos Lonicerae.4. ConclusionsThis is the first report on validation of an analytical method for qualification and quantification of saponins in Flos Lonicerae. This newly established HPLC-ELSD method can be used to simultaneously quantify seven saponins, i.e. macranthoidin B, macranthoidin A, dipsacoside B, hederagenin-28-O-β-D-glucopyranosyl(6→1)-O-β-D- glucopyranosyl ester, macranthoside B, macranthoside A, and hederagenin-3-O-α-L-arabinopyranosyl(2→1)-O-α-L-rhamnopyranoside in Flos Lonicerae. Together with the HPLC profiles of iridoids, the HPLC-ELSD profiles of saponins could also be used as an accessory chemical evidence to clarify the botanical origin and comprehensive quality evaluation of Flos Lonicerae.AcknowledgementsThis project is financially supported by Fund for Distinguished Chinese Young Scholars of the National Science Foundation of China (30325046) and the National High Tech Program(2003AA2Z2010).[1]Ministry of Public Health of the People’s Republic of China, Pharmacopoeia ofthe People’s Republic of China, V ol.1, 2000, p. 177.[2]W. Shi, R.B. Shi, Y.R. Lu, Chin. Pharm. J., 34(1999) 724.[3]J.B. Xing, P. Li, D.L. Wen, Chin. Med. Mater., 26(2001) 457.[4]Y.Q. Zhang, L.C. Xu, L.P. Wang, J. Chin. Med. Mater., 21(1996) 204.[5] D. Zhang, Z.W. Li, Y. Jiang, J. Pharm. Anal., 16(1996) 83.[6]T.Z. Wang, Y.M. Li, Huaxiyaoxue Zazhi, 15(2000) 292.[7]J.ZH. Shi, G.T. Liu. Acta Pharm. Sin., 30(1995) 311.[8]Y. P. Liu, J. Liu, X.SH. Jia, et al. Acta Pharmacol. Sin., 13 (1992) 209.[9]Y. P. Liu, J. Liu, X.SH. Jia, et al. Acta Pharmacol. Sin., 13 (1992) 213.[10]J.ZH. Shi, L. Wan, X.F. Chen.ZhongYao YaoLi Yu LinChuang, 6 (1990) 33.[11]J. Liu, L. Xia, X.F. Chen. Acta Pharmacol. Sin., 9 (1988) 395[12]H.J. Li, P. Li, W.C. Ye, J. Chromatogr. A 1008(2003) 167-72.[13]Q. Mao, D. Cao, X.SH. Jia. Acta Pharm. Sin., 28(1993) 273.[14]H. Kizu, S. Hirabayashi, M. Suzuki, et al. Chem. Pharm. Bull., 33(1985) 3473.[15]S. Saito, S. Sumita, N. Tamura, et al. Chem Pharm Bull., 38(1990) 411.[16]Alltech ELSD 2000 Operating Manual, Alltech, 2001, p. 16. In Chinese.[17]J.B. Xing, P. Li, Chin. Med. Mater., 22(1999) 366.Fig. 1 Chemical structures of seven saponins from Lonicera confusa macranthoidin B (1), macranthoidin A (2), dipsacoside B (3), hederagenin-28-O-β-D-glucopyranosyl(6→1)-O-β-D- glucopyranosyl ester (4), macranthoside B (5), macranthoside A (6), and hederagenin-3-O-α-L-arabinopyranosyl(2→1)-O-α-L-rhamnopyranoside (7)Fig. 2Representative HPLC chromatograms of mixed standards and methanol extracts of Flos Lonicerae.Column: Agilent Zorbax SB-C18 column(250 4.6mm, 5.0µm), temperature of 25℃; Detector: ELSD, drift tube temperature 106℃, nitrogen flow-rate 2.6 l/min.A: Mixed standards, B: L. confusa, C: L. japonica, D: L. macranthoides, E: L. hypoglauca, F: L. similes.Table 1 Calibration curves for seven saponinsAnalytes Calibration curve ar2Test range(μg)LOD(μg)LOQ(μg)1 y=6711.9x-377.6 0.9940 0.56–22.01 0.26 0.882 y=7812.6x-411.9 0.9922 0.54–21.63 0.26 0.843 y=6798.5x-299.0 0.9958 0.46–18.42 0.22 0.724 y=12805x-487.9 0.9961 0.38–15.66 0.10 0.345 y=4143.8x-88.62 0.9989 0.42–16.82 0.18 0.246 y=3946.8x-94.4 0.9977 0.40–16.02 0.16 0.207 y=4287.8x-95.2 0.9982 0.42–16.46 0.12 0.22a y: Peak area; x: concentration (mg/ml)Table 2 Reproducibility of the assayAnalyteIntra-day variability Inter-day variability Content (mg/g) Mean RSD (%) Content (mg/g) Mean RSD (%)1 46.1646.2846.2246.22 0.1346.2245.3647.4226.33 2.232 5.385.385.165.31 2.405.285.345.045.22 3.043 4.374.304.184.28 2.244.284.464.024.255.204 nd1)-- -- nd -- --5 1.761.801.821.79 1.701.801.681.841.77 4.706 1.281.241.221.252.451.241.341.201.26 5.727 tr2)-- -- tr -- -- 1): not detected; 2): trace. RSD (%) = (SD/Mean) ×100%Table 3 Recovery of the seven analytesAnalyteOriginal(mg) Spiked(mg)Found(mg)Recovery(%)Mean(%)RSD(%)1 23.0823.1423.1119.7122.8628.1042.7346.1351.0199.7100.699.399.8 0.722.692.672.582.082.913.164.735.515.7698.197.6100.698.8 1.632.172.152.091.732.182.623.884.404.6598.8103.297.799.9 2.94nd1)1.011.050.980.981.101.0297.0104.8104.1102.0 4.250.880.900.910.700.871.081.561.752.0197.197.7101.898.9 2.660.640.620.610.450.610.751.081.211.3397.796.796.096.8 0.97tr2)1.021.101.081.031.111.07100.9102.799.1100.9 1.81): not detected; 2): trace.a Recovery (%) = (Amount found –Original amount)/ Amount spiked ×100%, RSD (%) = (SD/Mean) ×100%Table 4 Contents of seven saponins in Lonicera spp.Content (mg/g)1 2 3 4 5 6 7 L. confusa45.65±0.32 5.13±0.08 4.45±0.11tr1) 2.04±0.04tr 1.81±0.03 L. japonica nd2)nd 3.44±0.09nd nd nd nd L. macranthoides46.22±0.06 5.31±0.13 4.28±0.10 tr 1.79±0.03 1.25±0.03 tr L. hypoglauca11.17±0.07 nq3)53.78±1.18nd 1.72±0.02 2.23±0.06 2.52±0.04 L. similes41.22±0.25 4.57±0.07 3.79±0.09nd 1.75±0.02tr nd 1): trace; 2): not detected.. 3) not quantified owing to the suspicious purity of the peak.。

CAS号413611-93-5_10074-G5_MedBio_物理性质

CAS号413611-93-5_10074-G5_MedBio_物理性质
CAS
1、产品物理参数:
常用名
10074-G5
英文名
10074-G5
CAS号
413611-93-5
分子量
332.313
密度
1.4±0.1 g/cm3
沸点
538.6±60.0 °C at 760 mmHg
分子式
C18H12N4O3
熔点
无资料
闪点
279.5±32.9 °C
2、技术资料:
体外研究
10074-G5抑制Daudi Burkitt淋巴瘤细胞的生长并破坏c-Myc / Max二聚化。针对Daudi和HL-60细胞的IC50值分别为15.6和13.5μM[1]。10074-G5在区域Arg363-Ile381中结合Myc肽Myc353-437,Kd值为2.8μM。10074-G5结合在由诱导螺旋结构域(Leu370-Arg378)的N末端的扭结(Asp379-Ile381)产生的空腔中[3]。
≥98%
品牌
货号
中文名称
英文名称
CAS
包装
纯度
MedBio
MED11457
CDK inhibitor II
CDK inhibitor II
1269815-17-9
50mg
≥98%
品牌
货号
中文名称
英文名称
CAS
包装
纯度
MedBio
MED11591
(S)-CCG-1423
(S)-CCG-1423
None
体内研究
静脉注射20 mg / kg小鼠的血浆半衰期为10074-G5,为37分钟,血药浓度峰值为58μM,比肿瘤峰值浓度高10倍[1]。
3、同类产品列表:

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

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]。

高效液相色谱法测定发酵液中3-羟基丁酮

高效液相色谱法测定发酵液中3-羟基丁酮

高效液相色谱法测定发酵液中3-羟基丁酮汤丹丹;王腾飞;王瑞明【摘要】The acetoin microorganism fermentation system was prepared by biological method. The method to determine acetoin by high performance liquid chromatography was studied. The fermentation broth was pre-treated by centrifuging and filtering with 0. 22 μm microporous membrane.A column of Hypersil NH2(300 mm × 4. 6 mm,5 μm)with an mobile phase containing acetonitrile and water(90∶10,V/V) was used for the analysis of acetoin in fermentation system,the flow rate was 1 mL/min,the column tem-perature and detector temperature was 35 ℃,the chromatography was completed in just 25 min. The re-covery rate was 95 . 96% ~101 . 2% and the relative standard deviations 1 . 69% ~2 . 09%. The method was proved to be a rapid and effective quantitative analysis method with simple pretreatment and high sen-sitive to determine the acetoin in fermentation broth,which was fit for guiding real-time monitoring the fermentation process.%针对生物法制备3-羟基丁酮的微生物发酵体系,研究了利用高效液相色谱法测定3-羟基丁酮的方法。

LCMS检测西他沙星原料中基因毒性杂质的含量

LCMS检测西他沙星原料中基因毒性杂质的含量

LC-MS检测西他沙星原料中基因毒性杂质的含量石莹1宋雪洁3李浩冬2路显锋2*1药物研究院分析所,扬子江药业集团,泰州2253212药物制剂新技术国家重点实验室,扬子江药业集团,泰州2253213质量管理部,扬子江药业集团,泰州225321摘要建立了LC-MS 法测定西他沙星中基因毒性杂质对甲苯磺酸甲酯和对甲苯磺酸乙酯含量的方法。

方法:采用Agilent Poroshell 120 EC-C18色谱柱;流动相为纯水(0.1%甲酸):甲醇(V/V)=60:40;稀释剂为乙腈(0.1%甲酸):纯水(V/V)=50:10;柱温为40℃;进样体积为5µl;流速为0.4ml/min;采用正离子模式进行扫描。

对甲苯磺酸甲酯测定浓度在0.76ng/ml~15.27ng/ml范围内,线性关系良好;对甲苯磺酸乙酯测定浓度在0.75ng/ml~15.01ng/ml范围内,线性关系良好。

对甲苯磺酸甲酯的定量限为0.0038ng;对甲苯磺酸乙酯的定量限为0.0038ng。

杂质回收率在限度浓度80%、100%和160%三个浓度水平均在90~110%之间,该方法准确度良好。

该方法适用于西他沙星原料中对甲苯磺酸甲酯和对甲苯磺酸乙酯的检测。

西他沙星(sitafloxacin)是日本第一制药有限公司继左氧氟沙星后开发出的一种强力广谱新氟喹诺酮类抗菌剂,该药对革兰氏阳性球菌,革兰氏阴性菌以及厌氧菌的抗菌活性是左氧氟沙星的4~32倍,同时对肺炎球菌DNA 促旋酶和拓扑同功酶有双重抑制作用。

临床表现有极广的抗菌谱,特别是对呼吸道的病菌有极强的抗菌活性。

因西他沙星的一个起始物料为对甲苯磺酸盐,在后续反应中对甲苯磺酸若有残留,可能会与溶剂甲醇、乙醇反应生成具有基因毒性的杂质—对甲苯磺酸甲酯和对甲苯磺酸乙酯,故采用LC-MS法对产品中的对甲苯磺酸甲酯/乙酯进行控制。

1、实验部分1.1仪器与试药Agilent 1200液相色谱仪(美国安捷伦公司);Agilent 6460三重串联四极杆质谱仪(美国安捷伦公司);XP205型电子天平(瑞士梅特勒托利多公司)。

QuEChERS前处理UPLC-MSMS(液质联用)法测定水产硝基呋喃代谢物

QuEChERS前处理UPLC-MSMS(液质联用)法测定水产硝基呋喃代谢物

482020/09中国食品工业彭 芸 珠海市食品药品检验所 广东珠海 519000QuEChERS 前处理UPLC-MS/MS(液质联用)法测定水产硝基呋喃代谢物摘要:本文实验中建立了一种用QuEChERS 前处理,用UPLC-MS/MS 测定水产中硝基呋喃代谢物的测定方法。

结果表明:在0.5~10.0ng/mL 范围内线性关系良好,r 均大于0.995;加标回收率范围在83.2%~108.9%,相对标准偏差( RSD)在2.2%~8.4%。

实验证明该方法具有过程简单、灵敏度高、回收率好等优点,可为水产中硝基呋喃代谢物的快速检测提供方法依据。

关键词:QuEChERS;硝基呋喃代谢物; UPLC-MS/MS法引言硝基呋喃类药物是人工合成的具有5-硝基呋喃结构的广谱抗菌药物,具有广谱抗菌作用,被广泛应用于医药、畜牧及水产养殖中防治细菌感染疾病。

[1]但该类药物半衰期很短,在动物体内能迅速代谢,而与蛋白结合的代谢物在生物体内能长期稳定残留,并具有潜在的致畸、致癌和诱导机体产生突变的作用。

[2]中华人民共和国农业农村部公告第250号将硝基呋喃列入《食品动物中禁止使用的药品及其他化合物清单》。

硝基呋喃类药物主要包括呋喃它酮、呋喃西林、呋喃妥因和呋喃唑酮,它们代谢物分别是5-吗啉甲基-3-氨基-2-噁唑烷基酮(AMOZ)、氨基脲(SEM)、1-氨基-2-内酰脲(AHD)和3-氨基-2-噁唑烷基酮(AOZ),这些代谢产物和蛋白质结合比较稳定, 能在生物组织中存留较长时间,故利用代谢物的检测可以反映硝基呋喃药物的残留状况。

[3]畜禽及水产品中硝基呋喃类代谢物的检测方法主要有免疫胶体金法、液相色谱法和液质联用法等。

监测动物性食品中残留的硝基呋喃类代谢物,目前最常用液质联用法,其前处理步骤相对简单、杂质干扰少,能够比较准确地对硝基呋喃类代谢1 作者简介:彭芸(1982—),女,学士,工程师;研究方向为食品安全。

物进行定性和定量分析。

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=====================================================================Acq. Operator : Wang Ke Cheng(LCMS-02) Seq. Line : 67
Acq. Instrument : HY-LCMS-02 Location : P1-A-06Injection Date : 1/19/2016 2:52:30 PM Inj : 1
Inj Volume : 3.000 µl
Acq. Method : D:\AGLIENT 1260\DATA\20160119\20160119 2016-01-19 09-05-10\100-1000MS+3MIN- 1.5_(0.02%FA).M
Last changed : 1/19/2016 9:05:10 AM by Wang Ke Cheng(LCMS-02)
Analysis Method : D:\AGLIENT 1260\DATA\20160119\20160119 2016-01-19 09-05-10\100-1000MS+3MIN- 1.5_(0.02%FA).M (Sequence Method)
Last changed : 1/19/2016 3:19:25 PM by Wang Ke Cheng(LCMS-02) (modified after loading)
Method Info : Postive,MS:100-1000,Column ID:A-RP-132,40℃
Catalog No : HY-13913 Batch#19277 A-RP-134
Additional Info : Peak(s) manually integrated
min
0.5
1
1.5
2 2.53mAU 0
20040060080010001200 DAD1 B, Sig=214,4 Ref=off (D:\AGLIENT 1260\DATA\20160119\20160119 2016-01-19 09-05-10\BIZ2016-119-WJ6.D)
1.889
1.995
2.163
2.240
===================================================================== Area Percent Report =====================================================================
Sorted By : Signal Multiplier : 1.0000Dilution : 1.0000
Do not use Multiplier & Dilution Factor with ISTDs
Signal 1: DAD1 B, Sig=214,4 Ref=off
Peak RetTime Type Width Area Height Area # [min] [min] [mAU*s] [mAU] %
----|-------|----|-------|----------|----------|--------| 1 1.889 MF 0.0761 2.00227 4.38580e-1 0.0520 2 1.995 FM 0.0757 2.75847 6.07104e-1 0.0716 3 2.163 MF 0.0282 3.21683 1.90048 0.0835 4 2.240 FM 0.0436 3846.11426 1468.76233 99.7930
Totals : 3854.09183 1471.70850
===================================================================== *** End of Report ***
=====================================================================Acq. Operator : Wang Ke Cheng(LCMS-02) Seq. Line : 67
Acq. Instrument : HY-LCMS-02 Location : P1-A-06Injection Date : 1/19/2016 2:52:30 PM Inj : 1
Inj Volume : 3.000 µl
Acq. Method : D:\AGLIENT 1260\DATA\20160119\20160119 2016-01-19 09-05-10\100-1000MS+3MIN- 1.5_(0.02%FA).M
Last changed : 1/19/2016 9:05:10 AM by Wang Ke Cheng(LCMS-02)
Analysis Method : D:\AGLIENT 1260\DATA\20160119\20160119 2016-01-19 09-05-10\100-1000MS+3MIN- 1.5_(0.02%FA).M (Sequence Method)
Last changed : 1/19/2016 2:50:56 PM by Wang Ke Cheng(LCMS-02) (modified after loading)
Method Info : Postive,MS:100-1000,Column ID:A-RP-132,40℃
Catalog No : HY-13913 Batch#19277 A-RP-134
Additional Info : Peak(s) manually integrated
min
0.5
1
1.5
2
2.5
3
20000
400006000080000100000 MSD1 TIC, MS File (D:\AGLIENT 1260\DATA\20160119\20160119 2016-01-19 09-05-10\BIZ2016-119-WJ6.D) ES-API, Pos, Scan
2.242
MS Signal: MSD1 TIC, MS File, ES-API, Pos, Scan, Frag: 50 Spectra averaged over upper half of peaks. Noise Cutoff: 1000 counts.
Reportable Ion Abundance: > 10%.
Retention Mol. Weight Time (MS) MS Area or Ion
2.242 181542 41
3.30 I 391.30 I 378.15 I 337.20 I 316.10 I 315.20 I 105.10 I 102.20 I
m/z
1002003004005006007000
204060
80100*MSD1 SPC, time=2.218:2.273 of D:\AGLIENT 1260\DATA\20160119\20160119 2016-01-19 09-05-10\BIZ2016-119-WJ6.D ES-API, Max: 20671
338.2
317.1
160.2
414.4
379.2
392.3
454.4
102.2
413.3
337.2
391.3
378.1
105.1
315.2
*** End of Report ***。

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