GSK2239633A-LCMS-32596-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。
碧云天(beyotime)生物产品代理目录价格表(2015年)
生物素3' 末端DNA标记试剂盒 生物素随机引物DNA标记试剂盒 D3308 化学发光法生物素标记核酸检测试剂盒 D3308B 封闭液(D3308专用) D3308W 洗涤液(5X，D3308专用)
产品名称
内切酶 产品编号 D6049 D6053 D6093 D6257 D6329 D6330 D6337 D6389 D6390 D6417 D6449 D6481 D6485 D6489 D6497 D6565 D6566 D6581 D6585 D6593 D6597 D6633 D6713 D6721 修饰酶 产品编号 D7012 D7021 D7027 D7035 D7039 D7051 D7062 D7066 D7069 D7073
1000U DNase I 100U RNase H Terminal Deoxynucleotidyl Transferase 500U 100U T4 Polynucleotide Kinase 500U T4 Polynucleotide Kinase 2000U BeyoRT M-MuLV反转录酶 2000U BeyoRT M-MuLV反转录酶(RNase H-) 产品名称 产品包装 2000U
ApaI BamHI BglII DpnI EcoRI EcoRI EcoRV HindIII HindIII KpnI MluI NcoI NdeI NheI NotI PstI PstI PvuII RsaI SacI SalI SmaI XbaI XhoI
产品名称
DNA末端平滑试剂盒 T4 RNA Ligase BeyoAP Alkaline Phosphatase Klenow Fragment Klenow Fragment，ExoT4 DNA Polymerase SP6 RNA Polymerase T3 RNA Polymerase T7 RNA Polymerase DNase I
封闭添加试剂(按字母顺序排列)
询价
4、BMPA
改变巯基基团为羧基基团，用于制备肽段-蛋白质交联物。
产品特点：
•反应基团：马来酰亚胺和羧基
•反应指向：巯基基团和胺（当与EDC结合使用时）
参考文献
Hermanson, G.T. (2008). Bioconjugate Techniques, 2nd ed., Elsevier Inc., pp.111-113. (Product # 20036)
25g
473
相关产品：
产品货号
产品名称
价格￥
24510
Sulfo-NHS
1848
22980
EDC
1005
20320
DCC
488
14、STAT，SATP和巯基添加试剂盒
添加保护性巯基防止二肽形成。
产品特点：
•与伯胺反应添加保护性巯基
•简单的脱保护步骤即可产生游离的巯基
•Thermo Scientific巯基添加试剂盒包含硫醇化作用，脱保护，纯化和定量所有需要的组分
订购信息：
产品货号
产品名称
包装
价格￥
23031
二盐酸乙二胺
10g
399
8、碘乙酰胺（Iodoacetamide），一次性使用
质谱前可靠的烷基化试剂。产品ຫໍສະໝຸດ 点：•与巯基基团形成共价键
•质谱级别（高纯度）
•方便，一次性使用形式（3个微型管，每管含有9.4mg）
•当用132μl碳酸氢铵（ammonium bicarbonate）溶解时，每管产生375mM的溶液
500mg
620
10、MMTS
可与巯基反应的可逆试剂。
产品特点：
•将-SH基团转化为-S-S-CH3
Sigma试剂清单
1.
缓冲液
产品货号 英文品名 中文品名 优惠价 (R M B ) 目录价 (RMB)
P6757-100G P6757-1KG P6757-25G P6757-500G PVP40-100G PVP40-1KG PVP40-500G PVP40-50G PVP40-5KG P1190-100G P1190-1KG P1190-500G P9666-100G P9666-1KG P9666-500G P5655-100G P5655-1KG P5655-500G P5629-10KG P5629-1KG P5629-25G P5629-500G S7545-1KG S7545-250G S7545-500G S3817-1KG S3817-500G S3817-5KG S7795-1KG S7795-500G S5886-10KG S5886-1KG S5886-500G S5886-5KG C8532-100G C8532-10KG C8532-1KG C8532-500G C8532-5KG S5136-100G S5136-1KG S5136-500G S5136-5KG S0751-100G S0751-1KG S0751-3KG S0751-500G T5816-100G T5816-1KG T5816-25G T5816-500G T6664-10PAK T1503-100G T1503-10KG T1503-1KG T1503-250G T1503-25G T1503-25KG T1503-500G T1503-50KG T1503-5KG
Ammonium acetate ~98% Ammonium acetate ~98% Ammonium acetate ~98% Boric acid Boric acid Carbonate-Bicarbonate Buffer Carbonate-Bicarbonate Buffer Citric acid trisodium salt Citric acid trisodium salt Citric acid trisodium salt Ethanolamine >=98% Ethanolamine >=98% Ethanolamine >=98% Ethanolamine >=98% Ethanolamine >=98% Ethylenediaminetetraacetic acid >=98.5% Ethylenediaminetetraacetic acid >=98.5% HEPES >=99.5% (titration) HEPES >=99.5% (titration) HEPES >=99.5% (titration) HEPES >=99.5% (titration) HEPES >=99.5% (titration) HEPES >=99.5% (titration) Imidazole >=98.5% (titration) Imidazole >=98.5% (titration) Imidazole >=98.5% (titration) Imidazole >=98.5% (titration) Imidazole >=98.5% (titration) Imidazole >=98.5% (titration) MES hydrate >=99.5% MES hydrate >=99.5% MES hydrate >=99.5% MES hydrate >=99.5% MOPS >=99.5% (titration) MOPS >=99.5% (titration) MOPS >=99.5% (titration) MOPS >=99.5% (titration) MOPS >=99.5% (titration) MOPS >=99.5% (titration) Phosphate buffered saline Phosphate buffered saline Phosphate-Citrate Buffer Phosphate-Citrate Buffer
GC测定盐酸普拉克索中三乙胺残留量
制霉菌素鱼肝油乳剂的制备与含量测定
医药导报 2006年 2月第 25卷第 2期
# 149#
管 中, 2 500 r# m in-1离心 30 m in, 结果无分层现象, 无油珠出现,
表 1 制霉菌素回收率实验结果
说明该制剂的物理稳 定性好。 3. 8. 2 有效期 预测 采用 初均 速法 测其稳 定性 [ 2], 将 制霉 菌
浓度
温度 / e
TK
1/t
t/h
55
328. 2
0. 003 047
7. 0
60
333. 2
0. 003 001
6. 0
65
338. 2
0. 002 957
5. 0
70
343. 2
0. 002 914
4. 0
75
348. 2
0. 002 872
3. 0
80
353. 2
0. 002 831
2. 0
85
358. 2
1. 样品溶液 2. 制霉菌素对照品溶液 3. 乳膏基质溶液 图 1 3种溶液的紫外扫描图谱
3. 5 样品测定 按处 方比 例配制 3批 次样 品, 精密 称取 样品 约 0. 2 g, 照 / 3. 50项下操作, 3批次样品中制霉菌素平均标示量 为 100. 73% , RSD 为 0. 56% ( n = 3)。 3. 6 稳定性考察 取 / 3. 50项下供试品溶液一份, 在配制后 1, 4, 6, 18, 24 h时测定制 霉菌素 含量, 结 果制霉 菌素 含量 RSD 为 0. 65% , 表明供试品溶液在 24 h内稳定。 3. 7 回收率实验 按处方比例配制 高 ( 120% )、中 ( 100% ) 、低 ( 80% ) 3个不同 浓度的供试 品, 分 别精密称取 约 0. 2 g 置于 50 mL容量瓶中, 加甲醇少许, 超声 振荡 2 m in使溶解, 加 甲醇至刻 度, 摇匀, 滤过, 弃去初滤液; 分别精密吸取续滤液 1 mL 置于 10 mL 容量瓶中, 加甲醇至刻度, 摇匀, 以甲醇为空白, 在 291 nm 波 长处分别测定吸光度, 计 算即得。 结果 见表 1。平 均回收 率为 100. 75% , RSD = 0. 87% 。 3. 8 稳定性考察 3. 8. 1 离心试验 取制霉菌素鱼 肝油乳 剂样品 1 g, 置 于离心
GSK3326595-SDS-MedChemExpress
Inhibitors, Agonists, Screening LibrariesSafety Data Sheet Revision Date:Oct.-08-2018Print Date:Oct.-08-20181. PRODUCT AND COMPANY IDENTIFICATION1.1 Product identifierProduct name :GSK3326595Catalog No. :HY-101563CAS No. :1616392-22-31.2 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)Skin corrosion ⁄irritation (Category 2),H315Serious eye damage ⁄eye irritation (Category 2A),H319Specific target organ toxicity, single exposure; Respiratory tract irritation (Category 3),H3352.2 GHS Label elements, including precautionary statementsPictogramSignal word WarningHazard statement(s)H315 Causes skin irritationH319 Causes serious eye irritationH335 May cause respiratory irritationPrecautionary statement(s)P261 Avoid breathing dust ⁄fume ⁄gas ⁄mist ⁄vapours ⁄spray.P305+P351+P338 IF IN EYES: Rinse cautiously with water for several minutes. Remove contact lenses, if present and easy to do.Continue rinsing.P302+352 IF ON SKIN: wash with plenty of soap and water.2.3 Other hazardsNone.3. COMPOSITION/INFORMATION ON INGREDIENTS3.1 SubstancesSynonyms:GSK-3326595;GSK 3326595Formula:C24H32N6O3Molecular Weight:452.55CAS No. :1616392-22-34. 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.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。
超高效液相色谱-静电场轨道阱高分辨质谱法测定法莫替丁及其制剂中的痕量N-亚硝基二甲胺
第39卷第9期ZO?。
年9月分析测试学报FENXI CESHI XUEBAO (Jon/ai af 1110/1116x 1:81 Analysis )Voi. 39 No 91779 〜DAdoi : 10. 3969/j. issn. 1004 -4457. 2020. 09. 003超高效液相色谱-静电场轨道阱高分辨质谱法测定法莫替丁及其制剂中的痕量N ■亚硝基二甲胺郭常川，杨书娟，刘 琦，王维剑，文松松，牛 冲，徐玉文**收稿日期：2722 -75 -21；修回日期：2722 -06 -21基金项目：国家自然科学基金项目(71573606, 71673076)*通讯作者：徐玉文，博士，主任药师，研究方向：药品检验，E - maii : *********************(山东省食品药品检验研究院国家药品监督管理局仿制药研究与评价重点实验室山东省仿制药一致性评价工程技术研究中心，山东济南250101)摘要：建立了测定法莫替丁及其制剂中N-亚硝基二甲胺(NDMA )含量的超高效液相色谱-静电场轨道阱高 分辨质谱法(UHPLC-Or/it/y HRMS)。
样品以甲醇作为提取溶剂，经涡旋混匀、恒温振荡、高速离心、微 孔过滤后进行液相色谱-质谱(LC - MS)分析。
采用ACE EXCEL 3氐-AR ( 164 mmx4.9 mm , 3 jm )色谱 柱，以0. 3%甲酸水溶液和0. 3%甲酸乙睛为流动相梯度洗脱分离，流速为0. 5。
mL/mm ,柱温为3。
C ,自 动进样器温度为4 C ,设置六通阀切换保护质谱系统。
质谱分析采用ESI 离子源，正离子平行反应监测 (PRM )扫描模式，外标法定量。
NDMA 在1.00~100.00 11/1^范围内线性良好，相关系数()为0.999 7,检 岀限和定量下限分别为0. 24 n/mL 和1. 00 n/mL ,在法莫替丁及其制剂中的平均回收率为98. 5% - 108% , 相对标准偏差(RSD )为2. 3% ~ 6. 7%。
乙酰胆碱酯酶抑制剂
上海应用技术学院研究生课程《高等天然产物化学》试卷2014 / 2015 学年第1 学期课程代码：NX0702013论文题目：乙酰胆碱酯酶抑制剂的研究进展姓名：芮银146061414康满满146061409专业：制药工程学院：化工学院乙酰胆碱酯酶抑制剂的研究进展芮银，陈祎桐，康满满摘要：本文阐述了乙酰胆碱酯酶抑制剂(AChEI)的研究进展，介绍了用于药物治疗的乙酰胆碱酯酶抑制剂的各种来源如植物、微生物等，及其抑制乙酰胆碱的活性物质。
在此基础上，总结了几种现代分析技术，对AChEIs进行筛选，大大加快AD药物资源的开发利用进程。
这些方法主要有基于比色法的Ellman's法及相关的改进方法、薄层显色法、荧光显色法、电喷雾质谱法等。
但是，到目前为止，现代分析技术在AD药物资源中的应用还处在起步阶段。
关键词：乙酰胆碱酯酶抑制剂，筛选方法，薄层显色法，荧光显色法The progress of acetylcholinesteraseinhibitorsRui Yin, Chen Yitong, Kang ManmanAbstract：In this artical, the research elaborates progress of acetylcholinesterase inhibitors (AChEI), and introduces a variety of sources for drug treatment acetylcholinesterase inhibitors such as plants, microorganisms, and its active ingredients. On this basis, the review summarizes several modern analytic techniques such as Ellman's method which based on the colorimetric method, TLC chromogenic method, fluorescent color method, Electrospray ionization mass spectrometry and so on. However, at present, the application of modern analytic techniques in AD drug resources is still in infancy.Key word: Acetylcholinesterase inhibitors, Screening Methods, TLC chromogenic method, Fluorescent color method目录摘要.................................................................................................错误!未定义书签。
基于反应体系的表面增强拉曼光谱快速检测乙基麦芽酚
基于反应体系的表面增强拉曼光谱快速检测乙基麦芽酚作者：吴昊肖东方应叶郭小玉文颖杨海峰来源：《上海师范大学学报·自然科学版》2020年第02期摘要：以鐵离子（Fe3+）为媒介，鞣酸还原氯金酸制备的金纳米粒子（Au NPs）作为表面增强拉曼散射（SERS）基底，实现比色一散射光谱双响应，快速鉴别食品中的乙基麦芽酚.其中比色法中，对乙基麦芽酚的检测限为0.50 mg·mL-1.SERS检测中，利用Fe3+和乙基麦芽酚的络合作用，乙基麦芽酚的最低检测限降低到0.01 mg ·mL-1，线性范围为0.05～1.00 mg·mL-1，该方法使用的仪器简单，操作方便，可对样品中的乙基麦芽酚进行现场直接测定，关键词：表面增强拉曼散射（SERS）;比色法;铁离子（Fe3+）;乙基麦芽酚中图分类号：0 657.37 文献标志码：A文章编号：1000-5137（2020）02-0167-080引言在食品中添加某些物质起到掩盖其不良品质的事件层出不穷，例如花生油掺假事件，这不仅意味着消费者权益受到损害，还往往伴随着食品质量不过关，严重危害消费者的健康.乙基麦芽酚是我国规定允许使用的食用香料，可作为烟草、饮料、糕点、香精、果酒、日用化妆品等物质的增香剂以及香味改良剂[l-2]，但大量摄入会导致头痛、呕吐，并可能影响肝功能和肾功能[3].因此，联合国粮食与农业组织和世界卫生组织食品添加剂专业委员会规定：乙基麦芽酚人均每天的摄入量以体重计不能超过2 mg·kg-1，而食品加工中的指导用量为100—200ug ·kg-1.目前，对于乙基麦芽酚的检测方法有气相色谱法[4]、高效液相色谱法[5]、荧光分析法[6]等，其中气相色谱方法相比于其他方法具有较高的准确性及灵敏度，但是针对复杂样品时，仍面临着前处理过程复杂、耗时长、需要大型检测仪器等缺点，而且乙基麦芽酚易挥发，限制了气相色谱检测方法在现场分析检测中的应用.近年来，随着便携式拉曼光谱仪器的飞速发展，使本就具有痕量分析检测[7-9]能力且样品前处理相对简单[10-11]的表面增强拉曼散射（ SERS）技术能实现现场快速无损检测，并被广泛应用于化学危害品、微生物污染物和生物毒素等的检测，本文作者设计了一种基于比色和表面增强拉曼光谱双响应的探针分子，用于食品中乙基麦芽酚的检测，图l为实验设计示意图.首先将铁离子（Fe3+）加入到待测溶液中，当待测体系中含有乙基麦芽酚这种物质时，会形成紫红色络合物，肉眼可直接辨别，此时Fe3+起到“固定”乙基麦芽酚分子的作用，再通过拉曼光谱进行检测，乙基麦芽酚特征峰出现，实现比色一散射光谱两种方式鉴别食品中的乙基麦酚.而当体系中不存在乙基麦芽酚或者乙基麦芽酚含量不足，导致Fe3+剩余时，剩余的Fe3+又与基底表面的鞣酸分子作用，使金纳米粒子（Au NPs）相互靠近，电磁场增强，引起“热点”增多，从而鞣酸信号增强，通过乙基麦芽酚特征峰强度的降低以及鞣酸特征峰信号的增强，可实现对乙基麦芽酚实现定量检测.1实验部分1.1试剂乙基麦芽酚购买于阿拉丁试剂公司，分析纯（AR）;罗丹明6G、氯金酸、氯化铁以及鞣酸均购置于国药试剂公司，均为AR;食用油从沃尔玛超市购买;实验中所用纯水均为自制的二次去离子水，所有的试剂和化学品均直接使用.实验玻璃仪器均用王水（浓盐酸和浓硝酸体积比为3：1混合）浸泡洗涤，再以二次去离子水冲洗.1.2仪器扫描电子显微镜（ SEM），S-4800型（Hitachi Co.，Ltd.）;7504紫外一可见分光光度仪，上海新茂仪器有限公司;ENWAVE（ Optronics） Prott-EZ-Raman-A2型便携式拉曼光谱仪，二极管激光器激发光波长为785 nm，其激发光源最大可调激光功率为300 mW，扫描时间为5s，累积时间为3次.1.3Au NPs的制备Au NPs的制备受SLOT等[12]工作的启发，以鞣酸为还原剂制备Au NPs.将3 mL质量分数为1%的氯金酸加入到100 mL三角烧瓶中，加入97 mL去离子水，煮沸15 min后，在剧烈搅拌条件下逐滴加入1.20 mL物质的量浓度为5xl0-3mol·L-1的鞣酸溶液，待溶液完全变成紫红色，停止加热并搅拌冷却至室温即可得到Au NPs.取8 mL上述Au纳米溶胶在8 000 r·min-I条件离心5 min，去掉上层清液，用去离子水洗涤2次后使用.1.4乙基麦芽酚纯品的测试称取0.10 g的乙基麦芽酚固体粉末加入10 mL容量瓶中，配置成质量浓度为10 mg· mL-1的母液，然后用去离子水逐步稀释成梯度浓度（7.500，5.000，2.500，1.000，0.750，0.500，0.250，0.100，0.075，0.050，0.010 mg·mL-1）溶液待用.将一定量Fe3+分别加入到不同质量浓度的乙基麦芽酚溶液中，使之反应形成络合物，然后取3 mL混合后的溶液与制备的Au NPs以1：1的体积比均匀混合，再取10 uL混合溶液滴在干净的铝箔上，待样品室温干燥后进行SERS测试.1.5实际样品中乙基麦芽酚的检测在进行实际检测时，由于乙基麦芽酚易溶于水，因此直接将Fe3+加入到5 mL食用油样品中，超声萃取5 min，然后取3 mL水层溶液与3 mL离心后的Au NPs充分混匀后，取10 uL混合后的溶液滴在干净的铝箔上，待样品室温干燥后进行SERS测试.作为实验对照，进行加标测试.向5 mL食用油样品中加入乙基麦芽酚，充分混匀后，按照上述步骤进行SERS测试.2结果与讨论2.1Au NPs的表征首先对制备的Au NPs进行了表征.图2（a）为Au NPs的SEM图，可以看出，Au NPs尺寸均一且分散均匀.图2（b）为Au NPs在521nm波长处产生吸收峰，根据公式可以计算出粒径在16 nm左右（Au NPs粒径公式：Y=0.401 7X+514.56，其中y为波长，X为粒子直径），可以看出这与图2（a）中的粒径大小相符.2.2 比色法检测乙基麦芽酚受LIU等[13]工作的启发，应用竞争反应原理，设计实行两步法快速、准确可视化地检测乙基麦芽酚，在本实验中，鞣酸以及乙基麦芽酚均可与Fe3+反应，但是鞣酸以及乙基麦芽酚对Fe3+的竞争能力相当，因此，当Fe3+与乙基麦芽酚发生反应时，鞣酸的引入不会破坏乙基麦芽酚与Fe3+生成的络合物.图3为比色法检测乙基麦芽酚（0，0.01，0.05.0.10.0.50，1.00，5.00 mg.mL-l），当乙基麦芽酚的质量浓度为0.50mg·mL-1时，可以观察到明显的颜色变化（溶液颜色从黄色变为紫红色）.溶液颜色随着溶液中乙基麦芽酚的浓度增加而加深，而当质量浓度低于0.50 mg·mL-l时，溶液的颜色就呈现出黄色.2.3Au NPs的SERS性能的考察由于SERS基底增强效果的好坏直接影响着测试结果的灵敏度，因此对制备的纳米粒子增强性能也作了考察，图4是以罗丹明6C为探针分子的鞣酸还原的Au NPs增强性能的SERS图谱，可以明显观测到罗丹明6G的特征峰，这是由于Au NPs的局域表面等离子体共振（LSPR），从而产生大量“热点”.该基底对罗丹明6G的检测限能达到5xl0-7 mol.L-l，灵敏度较好.2.4 乙基麦芽酚的SERS研究图5为乙基麦芽酚的SERS图谱与固体Raman图谱对比，可以观察到乙基麦芽酚的SERS 图谱与固体拉曼图谱几乎完全一致，无明显特征峰被选择性增强，因此猜测乙基麦芽酚在基底表面無特异性吸附作用.并利用高斯软件对乙基麦芽酚的SERS谱峰进行了归属，693 cm-1对应为乙基麦芽酚的Vs（C-O）以及Vs（C-C-C）振动模式，1034 cm-1对应为乙基麦芽酚的Vas （ C-O-C）以及Vas（C—C）振动模式，1 643 cm-1对应为Vs（C=C）以及8（C-O-H）振动模式.然而在不引入Fe3+的情况下进行乙基麦芽酚SERS直接测试时发现，由于乙基麦芽酚作为增香类食品添加剂，是一种挥发性小分子，在上述实验中也表明与基底无特异性作用，并且由于SERS测试时受环境温度及湿度影响较大，随着时间的延长，乙基麦芽酚的SERS信号也会随之发生变化.图6为在20℃，60%相对湿度条件下，2.50 mg.mL-1的乙基麦芽酚SERS强度随时间变化的图谱.从图6中可以看出，当不引入Fe3+时，孵育时间为38 min时会获得最佳信号，这不仅耗时长，还难以实现乙基麦芽酚的准确定量测定.同时，在不引入Fe3+的情况下，由于乙基麦芽酚与基底的非特异性吸附，乙基麦芽酚的最低可检测质量浓度为0.75 mg·mL-1，此方法的灵敏度不高，结果如图7所示.因此考虑使用Fe3+，将乙基麦芽酚“固定”下来进行检测，并首先对所用Fe3+浓度进行了实验.图8为Fe3+浓度测试结果.从图8中可以看出，当Fe3+物质的量浓度为0.16 mg·mL-l时，SERS信号最强.因此选择0.16 mg·mL-l的Fe3+为最佳浓度进行后续实验.当引入Fe“时，发现在l 339 cm-1以及l 479 cm-l处出现鞣酸的特征峰，当溶液中乙基麦芽酚浓度较低时，过量的Fe3+会与鞣酸结合，拉近Au NPs之间的距离，增强鞣酸的信号，SERS测试结果如图9所示，同时以1 034 cm-l处为乙基麦芽酚特征峰进行线性分析，结果如图lO（a）所示，此时线性范围为0.10～1.00 mg·mL-1.而当引入1339 cm-1鞣酸特征峰作为竞争因子时，以1 034 cm-l与1339 cm-1的比值进行线性分析时发现，最低可检测浓度为0.01 mg·mL-1，线性范围为0.05～1.00 mg/mL，线性范围更宽，结果如图lO（b）所示.2.5乙基麦芽酚实际样品的检测在模拟实际样品测试时，进行加标测试，分别向花生油中添加0.400 0 mg·mL-l和0.800 0 mg·mL-l的乙基麦芽酚，加标测试结果如表l所示.从表1中可以看出，回收率在89.90/0～103.5%之间，回收率良好.3结语引入Fe3+为媒介，Fe3+与乙基麦芽酚会形成紫红色络合物，实现颜色的初步判别，再以拉曼仪器进行测试乙基麦芽酚特征散射峰，实现比色一散射光谱两种方式鉴别食品中的乙基麦芽酚.而过量的Fe3+又会与基底表面的鞣酸作用，拉近Au NPs之间的距离，引起鞣酸特征峰的增强，通过乙基麦芽酚特征峰与鞣酸特征峰峰强的比值实现定量测试，不仅克服了挥发性小分子难以准确测定的难题，也降低乙基麦芽酚的最低检测浓度.在进行实际样品加标测试时，回收率在89.9%～103.5%之间，回收率良好.参考文献：[1] 杨小珊.气相色谱法测定食用植物油中乙基麦芽酚的含量[J].食品与发酵科技，2019，55（1）：119 - 121.YANG X S.Detenuination of ethyl maltol in edible vegetable oils by gas chromatography [J].Food and FermentationSciences&Technology， 2019，55（1）：119 - 121.[2] NI Y N，WANG Y，KOKOT S.Simultaneous kinetic-spectrophotometric determination ofmaltol and ethylmaltol in foodsamples by using chemometrics[J].Food Chemistry，2008， 109（ 2）：431 - 438.[3] 林灵超，吴方圆，高效液相色谱法同时测定牛奶中的香兰素与乙基香兰素[J].化学分析计量，2013，22（2）：60 - 62.2.2 比色法检测乙基麦芽酚受LIU等[13]工作的启发，应用竞争反应原理，设计实行两步法快速、准确可视化地检测乙基麦芽酚，在本实验中，鞣酸以及乙基麦芽酚均可与Fe3+反应，但是鞣酸以及乙基麦芽酚对Fe3+的竞争能力相当，因此，当Fe3+与乙基麦芽酚发生反应时，鞣酸的引入不会破坏乙基麦芽酚与Fe3+生成的络合物.图3为比色法检测乙基麦芽酚（0，0.01，0.05.0.10.0.50，1.00，5.00 mg.mL-l），当乙基麦芽酚的质量浓度为0.50mg·mL-1时，可以观察到明显的颜色变化（溶液颜色从黄色变为紫红色）.溶液颜色随着溶液中乙基麦芽酚的浓度增加而加深，而当质量浓度低于0.50 mg·mL-l时，溶液的颜色就呈现出黄色.2.3Au NPs的SERS性能的考察由于SERS基底增强效果的好坏直接影响着测试结果的灵敏度，因此对制备的纳米粒子增强性能也作了考察，图4是以罗丹明6C为探针分子的鞣酸还原的Au NPs增强性能的SERS图谱，可以明显观测到罗丹明6G的特征峰，这是由于Au NPs的局域表面等离子体共振（LSPR），从而产生大量“热点”.该基底对罗丹明6G的检测限能达到5xl0-7 mol.L-l，灵敏度较好.2.4 乙基麦芽酚的SERS研究图5为乙基麦芽酚的SERS图谱与固体Raman图谱对比，可以观察到乙基麦芽酚的SERS 图谱与固体拉曼图谱几乎完全一致，无明显特征峰被选择性增强，因此猜测乙基麦芽酚在基底表面无特异性吸附作用.并利用高斯软件对乙基麦芽酚的SERS谱峰进行了归属，693 cm-1对应为乙基麦芽酚的Vs（C-O）以及Vs（C-C-C）振动模式，1034 cm-1对应为乙基麦芽酚的Vas （ C-O-C）以及Vas（C—C）振动模式，1 643 cm-1对应为Vs（C=C）以及8（C-O-H）振动模式.然而在不引入Fe3+的情况下进行乙基麦芽酚SERS直接测试时发现，由于乙基麦芽酚作为增香类食品添加剂，是一种挥发性小分子，在上述实验中也表明与基底无特异性作用，并且由于SERS测试时受环境温度及湿度影响较大，随着时间的延长，乙基麦芽酚的SERS信号也会随之发生变化.图6为在20℃，60%相对湿度条件下，2.50 mg.mL-1的乙基麦芽酚SERS强度随时间变化的图谱.从图6中可以看出，当不引入Fe3+时，孵育时间为38 min时会获得最佳信号，这不仅耗时长，还难以实现乙基麦芽酚的准确定量测定.同时，在不引入Fe3+的情况下，由于乙基麦芽酚与基底的非特异性吸附，乙基麦芽酚的最低可检测质量浓度为0.75 mg·mL-1，此方法的灵敏度不高，结果如图7所示.因此考虑使用Fe3+，将乙基麦芽酚“固定”下来进行检测，并首先对所用Fe3+浓度进行了实验.图8为Fe3+浓度测试结果.从图8中可以看出，当Fe3+物质的量浓度为0.16 mg·mL-l时，SERS信号最强.因此选择0.16 mg·mL-l的Fe3+为最佳浓度进行后續实验.当引入Fe“时，发现在l 339 cm-1以及l 479 cm-l处出现鞣酸的特征峰，当溶液中乙基麦芽酚浓度较低时，过量的Fe3+会与鞣酸结合，拉近Au NPs之间的距离，增强鞣酸的信号，SERS测试结果如图9所示，同时以1 034 cm-l处为乙基麦芽酚特征峰进行线性分析，结果如图lO（a）所示，此时线性范围为0.10～1.00 mg·mL-1.而当引入1339 cm-1鞣酸特征峰作为竞争因子时，以1 034 cm-l与1339 cm-1的比值进行线性分析时发现，最低可检测浓度为0.01 mg·mL-1，线性范围为0.05～1.00 mg/mL，线性范围更宽，结果如图lO（b）所示.2.5乙基麦芽酚实际样品的检测在模拟实际样品测试时，进行加标测试，分别向花生油中添加0.400 0 mg·mL-l和0.800 0 mg·mL-l的乙基麦芽酚，加标测试结果如表l所示.从表1中可以看出，回收率在89.90/0～103.5%之间，回收率良好.3结语引入Fe3+为媒介，Fe3+与乙基麦芽酚会形成紫红色络合物，实现颜色的初步判别，再以拉曼仪器进行测试乙基麦芽酚特征散射峰，实现比色一散射光谱两种方式鉴别食品中的乙基麦芽酚.而过量的Fe3+又会与基底表面的鞣酸作用，拉近Au NPs之间的距离，引起鞣酸特征峰的增强，通过乙基麦芽酚特征峰与鞣酸特征峰峰强的比值实现定量测试，不仅克服了挥发性小分子难以准确测定的难题，也降低乙基麦芽酚的最低检测浓度.在进行实际样品加标测试时，回收率在89.9%～103.5%之间，回收率良好.参考文献：[1] 杨小珊.气相色谱法测定食用植物油中乙基麦芽酚的含量[J].食品与发酵科技，2019，55（1）：119 - 121.YANG X S.Detenuination of ethyl maltol in edible vegetable oils by gas chromatography [J].Food and FermentationSciences&Technology， 2019，55（1）：119 - 121.[2] NI Y N，WANG Y，KOKOT S.Simultaneous kinetic-spectrophotometric determination ofmaltol and ethylmaltol in foodsamples by using chemometrics[J].Food Chemistry，2008， 109（ 2）：431 - 438.[3] 林灵超，吴方圆，高效液相色谱法同时测定牛奶中的香兰素与乙基香兰素[J].化学分析计量，2013，22（2）：60 - 62.。