_1S,3R,5R_-PIM447_dihydrochloride_LCMS_23225_MedChemExpress
ACCUSPIN系统-Histopaque 1077产品说明书
Technical BulletinACCUSPIN™ System – Histopaque ® 1077Catalog Numbers A6929, A7054, and A0561Product DescriptionACCUSPIN System-Histopaque -1077products are intended for use in the isolation of lymphocytes and other mononuclear cells. The separation medium, Histopaque-1077, is a sterile-filtered, endotoxin tested solution of polysucrose and sodium diatrizoate, adjusted to a density of 1.077 g/mL. The ACCUSPIN tube is specially designed with two chambers separated by a porous high density polyethylene barrier (frit).Separation of lymphocytes and other mononuclear cells from whole blood and bone marrow using density gradientseparation media is based on a published method.1 Histopaque-1077 is suitable for human lymphocyte antigen (HLA) typing 2 and as the initial isolation step prior toenumeration of T, B, and ‘null’ lymphocytes.3 It may also be employed in the preparation of pure lymphocyte suspensions for cell culture and cytotoxicity assays.4ACCUSPIN System-Histopaque-1077 products consist of radiation sterilized polypropylene tubes fitted with a highdensity polyethylene frit and aseptically filled with Histopaque-1077.Histopaque-1077 is a sterile-filtered solution of polysucrose, 57 g/L, and sodium diatrizoate, 90 g/L.Density: 1.076–1.078 g/mL Endotoxin: 0.3 EU/mL pH: 8.8–9.0ACCUSPIN System-Histopaque-1077Catalog No. A692940 × 3 mLEach tube contains 3 mL ofHistopaque 1077-1 and will separate 3-6 mL of anticoagulated blood Catalog No. A7054 12 × 15 mLCatalog No. A0561100 × 15 mLEach tube contains 15 mL ofHistopaque 1077-1 and will separate 15-30 mL of anticoagulated bloodReagents and Equipment Required but Not ProvidedCentrifuge (swinging bucket rotor)capable of generating 100 to 1,000 g Centrifuge tubes for washing mononuclear cellsIsotonic phosphate buffered saline solution or appropriate cell culture mediumPrecautions and DisclaimerFor R&D use only. Not for drug, household, or other uses. Please consult the Safety Data Sheet for information regarding hazards and safe handling practices.Preparation InstructionsSpecimen Collection - Collect blood in preservative-free anticoagulant (EDTA or heparin) or use defibrinated blood. For best results, blood should be processed within 2 hours.On occasion, it may be necessary to dilute the blood sample 3 to 5-fold, depending on absolute cell numbers. A similar volume of prediluted blood may be used or the blood sample may be diluted directly in upper chamber of the ACCUSPIN tube (seeProcedure, step 3). This is appropriate for specimens with hematocrits above normal.Storage/StabilityStore the products at 2–8 C.Histopaque-1077 has an expiration period of 3 years. Reagent label bears expiration date.ProcedureAnticoagulated blood can be added to the top chamber of the tube without risk of mixing with the Histopaque-1077 in the lowerchamber under the frit. On centrifugation the whole blood migrates through the frit to contact with the Histopaque-1077. The elements of greater density displace a volume of Histopaque-1077 above the frit giving a clear separation of the bloodcomponents. The erythrocytes aggregate and the granulocytes become slightly hypertonic, increasing their sedimentation rate, resulting in pelleting at the bottom of the ACCUSPIN Tube. Lymphocytes and other mononuclear cells, e.g., monocytes, remain at the plasma/Histopaque-1077 interface. This dense band of mononuclear cells may be collected by pouring off the contents of the upper chamber or by means of a pipette. Erythrocyte contamination is avoided due to the barrier between the chambers.Most extraneous platelets are removed by low speed centrifugation during the washing steps.1. Bring desired number of tubes to roomtemperature. If Histopaque-1077 isabove the frit prior to use, centrifuge at 1,000 g for 30 seconds at room temperature.Note: Failure to bring ACCUSPIN System-Histopaque-1077 to room temperature may cause limited recovery of mononuclear cells. 2. Label tube(s).3. Freely pour the blood sample into theupper chamber of each ACCUSPIN System-Histopaque-1077 tube.a. Use 3–6 mL of whole blood withACCUSPIN System-Histopaque-1077 tubes, Catalog No. A6929. b. Use 15–30 mL of whole blood withACCUSPIN System-Histopaque-1077 tubes, Catalog Nos. A7054 or A0561. Note: Use of volumes of prediluted or whole blood other than those recommended may result in decreased recovery.4. Centrifuge at 1,000 g for 10 minutes atroom temperature or centrifuge at 800 g for 15 minutes at roomtemperature. Centrifugation at lower temperatures, such as 4 C, may result in cell clumping and poor recovery.Note: If platelet contamination is a concern, add the mononuclear cells to a 4-20% sucrose gradient that has been layered over Histopaque-1077.Centrifuge at 1,000 × g for 10 minutes at room temperature. The platelets will pellet at the bottom, while themononuclear cells will migrate to the Histopaque-1077 layer.5. After centrifugation, carefully aspiratethe plasma layer with a Pasteur pipette to within 0.5 cm of the opaque interface containing mononuclear cells. Properly dispose of the plasma layer.Note: Failure to remove the excesssupernatant may result in contamination of the mononuclear band with plasma proteins.6. Carefully transfer the opaque interfacewith a Pasteur pipette into a clean conical centrifuge tube.Note: Removal of Histopaque-1077 with the mononuclear band increasesgranulocyte contamination from residual granulocytes, which may remain at the mononuclear interface.7. Wash the cells by adding 10 mL ofisotonic phosphate buffered saline solution or appropriate cell culture medium and mix by gently drawing in and out of a Pasteur pipette. 8. Centrifuge at 250 g for 10 minutes. 9. Aspirate the supernatant and discard. 10. Resuspend cell pellet with 5 mL ofisotonic phosphate buffered saline solution or appropriate cell culture medium and mix by gently drawing in and out of a Pasteur pipette.11. Centrifuge at 250 g for 10 minutes. 12. Repeat steps 9, 10, and 11, discardsupernatant and resuspend cell pellet in 0.5 mL of isotonic phosphate buffered saline solution or appropriate cell culture medium. Erythrocytes and granulocytes should pellet to the bottom of the ACCUSPIN tube. Mononuclear cells should band at the interface between the Histopaque-1077 and the plasma. If observed results vary from expected results, please contact Sigma-Aldrich Technical Service for assistance.References1. Boyum, A., Separation of leukocytesfrom blood and bone marrow. Scand. J. Clin. Lab. Invest ., 21 (Suppl 97), 77 (1968).2. Amos, D.B., and Pool, P., “HLA typing” inManual of Clinical Immunology, Rose, N.R., and Friedman, H., eds., American Society for Microbiology, (Washington, DC: 1976) pp. 797-804.3. Winchester, R.J., and Ross, G., “Methodsfor enumerating lymphocyte populations” in Manual of Clinical Immunology, Rose, N.R., and Friedman, H. eds., American Society for Microbiology, (Washington, DC: 1976) pp. 64-76.4. Thorsby, E., and Bratlie, A., “A rapidmethod for preparation of pure lymphocyte suspensions.”Histocompatibility Testing, Terasaki, P.I., ed., 665-666 (1970).The life science business of Merck operates as MilliporeSigma in the U.S. and Canada.Merck, Sigma-Aldrich, ACCUSPIN, and Histopaque are trademarks of Merck KGaA, Darmstadt, Germany or its affiliates. All other trademarks are the property of their respective owners. Detailed information on trademarks is available via publicly accessible resources.© 2022 Merck KGaA, Darmstadt, Germany and/or its affiliates. All Rights Reserved.NoticeWe provide information and advice to our customers on application technologies and regulatory matters to the best of our knowledge and ability, but without obligation or liability. Existing laws and regulations are to be observed in all cases by our customers. This also applies in respect to any rights of third parties. Our information and advice do not relieve our customers of their own responsibility for checking the suitability of our products for the envisaged purpose.The information in this document is subject to change without notice and should not be construed as a commitment by the manufacturing or selling entity, or an affiliate. We assume no responsibility for any errors that may appear in this document.Contact InformationFor the location of the office nearest you, go to /offices .Technical ServiceVisit the tech service page on our web site at /techservice .Standard WarrantyThe applicable warranty for the products listed in this publication may be found at /terms .A0561 Technical Bulletin Rev 06/2022。
小鼠肺癌原位模型的建立
小鼠肺癌原位模型的建立Establishment of orthotopic lung cancer model in mice XU Zihang LIU Fei ZOU Chunpu ZHU Shiguo CHEN XiaoSchool of Basic Medical Science ，Shanghai University of Traditional Chinese Medicine ，Shanghai 201203 ，China[] Objective Morbidity and mortality remain high in lung cancer ，but the animal lung cancer models used for the experimental research are limited ，so to establish an orthotopic lung cancer model，which is stable and similar to the human tumor microenvironment ，is a foundation for the further study of lung cancer research. Methods Luciferase-expressed LLC cells and matrigel matrix were directly injected into the left lung of C57BL/6 mice after cutting open a incision of the skin ，which about 1 cm ，and there was no need to open the chest. Small animal in vivo bioluminescence imaging system was used to monitor tumor growth and metastasis. At different time points ，mice were sacrificed and the lung tissues were isolated and imbedded with paraffin. Pathological diagnosis was madebysliced and HEstained. Results LLC cells (0.5 x 105) were enough to form an orthotopic pulmonary tumor ，and the success rate wasabove 90%. The metastases to contralateral thoracic ，contralateral lung ，bilateral axillary and inguinal lymph nodes were monitored by bioluminescence technique. Conclusion The orthotopic tumor models of lung cancer can successfully built by injection ofluciferase-expressed LLC cells and matrigel matrix mixture. Furthermore ，a few LLC cells are needed ，and the tumor formation rate is high ，besides there is no operation death risk. It has good metastases and high repeatability ，in addition it's easy to operate and easy to be monitored ，which provides a good method for the establishment of mouse models for further study of lung cancer.目前，肺癌动物模型的构建方法有化学诱导法、转基因法、异位移植法、原位移植法等。
《中国药典》(2020年版)复方磺胺恶唑片中的甲氧苄啶含量测
《中国药典》(2020年版)复方磺胺噁唑片中的甲氧苄啶含量测甲氧苄啶（Trimethoprim, TMP），又称为甲氧苄氨嘧啶、甲氧苄嘧啶，是一种抗菌增效药，与磺胺类药物联合使用时，能使磺胺类药物抗菌谱扩大、抗菌活性大大增强。
由于其独特的作用，甲氧苄啶在养殖业病害防治中被广泛应用。
迪信泰检测平台采用高效液相色谱(HPLC)和液相色谱-三重四极杆质谱(LC-MS/MS)法，可高效、精准的检测甲氧苄啶的含量变化。
此外，我们还提供其他抗生素检测服务，以满足您的不同需求。
HPLC和LC-MS测定甲氧苄啶样本要求：1. 请确保样本量大于0.2g或者0.2mL。
周期：2~3周项目结束后迪信泰检测平台将会提供详细中英文双语技术报告，报告包括：1. 实验步骤（中英文）2. 相关质谱参数（中英文）3. 质谱图片4. 原始数据5. 甲氧苄啶含量信息应用范围：本方法采用高效液相色谱法测定复方磺胺甲恶唑片中磺胺甲恶唑和甲氧苄啶的含量。
本方法适用于复方磺胺甲恶唑片。
方法原理：供试品加甲醇稀释，最终用流动相定量稀释后，进入高效液相色谱仪进行色谱分离，用紫外吸收检测器，于波长240nm处检测磺胺甲恶唑和甲氧苄啶的吸收值，计算出其含量。
试剂： 1. 0.1mol/L盐酸2. 乙腈3. 三乙胺4. 氢氧化钠试液5. 冰醋酸仪器设备： 1. 仪器1.1 高效液相色谱仪1.2 色谱柱十八烷基硅烷键合硅胶为填充剂，理论塔板数按磺胺甲恶唑峰计算不低于4000。
磺胺甲恶唑和甲氧苄啶的分离度应符合要求。
1.3 紫外吸收检测器2. 色谱条件2.1 流动相：水乙腈三乙胺=799 200 1（用氢氧化钠试液或冰醋酸调节pH 值至5.9。
）2.2 检测波长：240nm2.3 柱温：室温试样制备：1. 称取供试品取本品10片，精密称定，研细，精密称取适量（约相当于磺胺甲恶唑44mg）置100mL量瓶中。
2. 对照品溶液的制备精密称取磺胺甲恶唑对照品和甲氧苄啶对照品适量，用0.1mol/L盐酸溶液溶解并定量稀释制成每1mL中约含有磺胺甲恶唑0.44mg的和甲氧苄啶89µg的溶液。
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。
medip实验流程
medip实验流程English Response:MeDIP-seq (Methylated DNA Immunoprecipitation sequencing) is an experimental technique used to identify and characterize methylated regions of DNA. It involves immunoprecipitating methylated DNA fragments using an antibody specific to 5-methylcytosine (5mC), followed by sequencing the precipitated DNA.Key steps in the MeDIP-seq workflow:1. DNA fragmentation: Genomic DNA is fragmented using sonication or enzymatic digestion to generate DNA fragments of an appropriate size for immunoprecipitation.2. Immunoprecipitation: Fragmented DNA is incubated with an antibody specific to 5mC. The methylated DNA fragments are immunoprecipitated using magnetic beads or protein A/G beads conjugated to the antibody.3. DNA library preparation: Immunoprecipitated DNA is purified and used to generate a DNA library for sequencing. This typically involves end-repair, dA-tailing, andligation of sequencing adapters.4. Sequencing: The DNA library is sequenced using a next-generation sequencing platform.5. Data analysis: Sequencing reads are aligned to the reference genome, and bioinformatic tools are used to identify methylated regions and analyze methylation patterns.MeDIP-seq provides valuable insights into the epigenetic landscape of the genome. It has been widely used to study DNA methylation in various biological contexts, including development, disease, and environmental exposure.中文回答：MeDIP 实验流程。
高效液相色谱-串联质谱法检测泮托拉唑钠原料药中的水合肼
·药物研发·高效液相色谱-串联质谱法检测泮托拉唑钠原料药中的水合肼赵会明 张振洋 樊华军［英格尔检测技术服务（上海）有限公司 上海 201100］摘要建立了泮托拉唑钠原料药中的基因毒性杂质水合肼的高效液相色谱-串联质谱（LC-MSMS）检测方法。
采用反相色谱，以水-乙腈（含0.1%甲酸）为流动相，梯度洗脱，流速0.5 mL/min，以ESI正离子多反应监测（MRM）模式进行质谱检测。
结果显示，水合肼的检测限和定量限可达到0.23、0.47 ng/mL，其在0.47~9.37 ng/mL浓度范围内线性关系良好（r=0.999 9），准确度试验中低、中、高浓度回收率均在81.6%~90.9%之间。
在3批次泮托拉唑钠原料药中均未检出水合肼。
关键词高效液相色谱-串联质谱法基因毒性杂质泮托拉唑钠水合肼痕量检测中图分类号：R917; O657 文献标志码：A 文章编号：1006-1533(2022)11-0072-04引用本文 赵会明, 张振洋, 樊华军. 高效液相色谱-串联质谱法检测泮托拉唑钠原料药中的水合肼[J]. 上海医药, 2022, 43(11): 72-75.Determination of hydrazine hydrate in pantoprazole sodium by high performance liquid chromatography-tandem mass spectrometryZHAO Huiming, ZHANG Zhenyang, FAN Huajun[ICAS Testing Technology Service (Shanghai) CO., LTD., Shanghai 201100, China]ABSTRACT To establish a high-performance liquid chromatography-tandem mass spectrometry (LC-MSMS) method for the determination of hydrazine hydrate in active pharmaceutical ingredient (API) pantoprazole sodium. HPLC was carried out by reverse chromatography using water-acetonitrile containing 0.1% formic acid as flow phase and gradient elution at a flow rate of 0.5 mL/min. Mass spectrometry was performed with multi-reaction monitoring (MRM) in positive ESI mode. The detection and quantitative limits of hydrazine hydrate reached 0.23, 0.47 ng/mL and hydrazine hydrate showed good linear relationship in the range of 0.47-9.37 ng/mL (r=0.999 9). The recoveries of samples at low, medium and high-level concentrations reached81.6% to 90.9% in the accuracy experiment. No hydrazine hydrate was detected in 3 batches of pantoprazole sodium.KEY WORDS HPLC-tandem mass spectrometry; genotoxic impurities; pantoprazole sodium; hydrazine hydrate; trace determination上消化道出血是近年的临床疾病中常见且多发的一种疾病，其临床表现为呕血、黑便等，如得不到及时有效治疗，可能引发失血性休克。
双联频那醇硼酸酯检测方法
双联频那醇硼酸酯检测方法
双联频那醇硼酸酯（Bis(pinacolato)diboron）是一种有机硼化合物，主要用于药物合成和有机催化等领域。
检测双联频那醇硼酸酯的方法有很多种，以下是一些常用的方法：
1. 核磁共振氢谱（1H-NMR）：这是一种常用的结构鉴定方法，通过分析化合物的氢原子信号，可以确定双联频那醇硼酸酯的结构。
2. 质谱（MS）：质谱是通过分析化合物的质量来鉴定其结构的。
双联频那醇硼酸酯的质谱通常包括分子离子峰、碎片离子峰等，可以用于确定其分子量和结构。
3. 红外光谱（IR）：红外光谱是通过分析化合物的红外吸收光谱来鉴定其结构的。
双联频那醇硼酸酯的红外光谱通常包括C=O、C-H、B-O等键的吸收峰，可以用于确定其结构。
4. 紫外光谱（UV）：紫外光谱是通过分析化合物的紫外吸收光谱来鉴定其结构的。
双联频那醇硼酸酯的紫外光谱通常包括苯环、酮基等官能团的吸收峰，可以用于确定其结构。
5. 高效液相色谱（HPLC）：高效液相色谱是一种常用的分离和
检测方法。
通过将双联频那醇硼酸酯与其他化合物分离，然后用紫外检测器或质谱检测器检测其含量，可以实现对其的定量分析。
6. 元素分析：元素分析是通过分析化合物中元素的种类和含量来鉴定其结构的。
双联频那醇硼酸酯的元素分析主要包括碳、氢、硼等元素的测定。
这些方法可以根据实际需要和样品特性进行选择和组合，以实现对双联频那醇硼酸酯的准确检测。
鹅掌柴蜂蜜中特征性成分鉴定及真实性评价
王琪琦，黄忠连，王莉，等. 鹅掌柴蜂蜜中特征性成分鉴定及真实性评价[J]. 食品工业科技，2023，44（23）：238−245. doi:10.13386/j.issn1002-0306.2022100052WANG Qiqi, HUANG Zhonglian, WANG Li, et al. Characteristic Compounds Identification and Authenticity Evaluation of Heptapleurum Honey[J]. Science and Technology of Food Industry, 2023, 44(23): 238−245. (in Chinese with English abstract). doi:10.13386/j.issn1002-0306.2022100052· 分析检测 ·鹅掌柴蜂蜜中特征性成分鉴定及真实性评价王琪琦1,2，黄忠连3，王 莉4，董 捷2，林 珣2，张根生1, *（1.哈尔滨商业大学食品工程学院，黑龙江哈尔滨 150000；2.中国农业科学院蜜蜂研究所，北京 100093；3.广西梧州甜蜜家蜂业有限公司，广西梧州 543000；4.江苏鸿祺生物科技有限公司，江苏泰州 225300）摘 要：为明确鹅掌柴蜂蜜中特征性成分并建立鹅掌柴蜂蜜的真实性评价方法，本研究采用高效液相色谱-四极杆飞行时间串联质谱（HPLC-Q-TOF-MSMS ）法对鹅掌柴蜂蜜中特征性成分进行定性定量分析。
在鹅掌柴蜂蜜中共鉴定出5个成分，分别为4-(1’-环乙醚-3’-丁二醇)-3,5,5-三甲基-2-环己烯酮（苦蜜素B ）、3,4,5-三甲氧基苯丙烯醇、4-(1’2’-二羟基-3’环氧丙烷)-3,5,5-2-环己烯酮（苦蜜素C ）、反,反式脱落酸、顺,反式脱落酸。
其中首次在蜂蜜中发现3,4,5-三甲氧基苯丙烯醇，并将其定为鹅掌柴蜂蜜的标志性成分。