AZD1208_LCMS_13429_MedChemExpress
高效液相色谱法测定磺达肝癸钠注射液清洁验证残留物含量
高效液相色谱法测定磺达肝癸钠注射液清洁验证残留物含量发布时间：2021-01-13T14:11:07.717Z 来源：《医师在线》2020年9月18期作者：吴萍黄皆竣石小磊蒋红梅[导读] 采用高效液相色谱法测定磺达肝癸钠注射液清洁验证残留物含量吴萍黄皆竣石小磊蒋红梅（扬子江药业集团江苏紫龙药业有限公司；江苏常州213000）摘要目的：采用高效液相色谱法测定磺达肝癸钠注射液清洁验证残留物含量方法：色谱柱：Dionex CarboPacTM PA1预柱，Dionex CarboPacTM PA1色谱柱，4×250mm；柱温：25℃；1.0ml/min；检测波长：210nm；进样量：100μl；流动相：流动相A为二甲亚砜磷酸盐缓冲液溶液【1000ml磷酸盐缓冲液中加入约15±10μl二甲亚砜，如基线产生正相漂移，则增加二甲亚砜的用量，反之则减少二甲亚砜的用量，二甲亚砜的实际用量为5~25μl不等】；流动相B为2.0mol/L氯化钠磷酸盐缓冲液溶液【取0.210g磷酸二氢钠二水物和0.650g磷酸氢二钠二水物用水溶解，然后稀释至1000ml，用磷酸调节溶液pH约为7.3】。
结果：磺达肝癸钠注射液清洁验证残留物磺达肝癸钠在12.9088μg/ml -161.36μg/ml范围内线性关系良好，不锈钢板的平均回收率在70%，RSD值为18%。
结论：本方法稳定、简便、准确，灵敏度高，适用于磺达肝癸钠注射液清洁验证残留物的含量测定。
正文：磺达肝癸钠注射液，西药名。
为抗血栓形成药。
用于进行下肢重大骨科手术如髋关节骨折、重大膝关节手术或者髋关节置换术等患者，预防静脉血栓栓塞事件的发生等。
在药品生产过程中，为防止污染与交叉污染，需对涉及的生产设备进行清洁，为保证清洁的有效性，需对设备表面化学残留物进行检测，本文建立了高效液相色谱法测定磺达肝癸钠注射液清洁验证残留量。
1 仪器和试药Agilent Infinity II 生物惰性色谱仪磺达肝癸钠对照品（WSFS-191201，5.0425mg/ml）；二甲亚砜（20181205，99.8%）；磷酸二氢钠（20190116，99.0%）；磷酸氢二钠（20170401，99.0%）；氯化钠（K5072204913）；2 方法与结果2.1 溶液的配制2.1.1 对照品溶液的制备取磺达肝癸鈉对照品一支（标定浓度约5mg/ml），精密量取0.4ml，置25.0ml量瓶中，加水溶解并稀释至刻度，摇匀，作为对照品溶液。
HSF1A_DataSheet_MedChemExpress
Inhibitors, Agonists, Screening Libraries Data SheetBIOLOGICAL ACTIVITY:HSF1A is a cell–permeable activator of heat shock transcription factor 1 (HSF1).IC50 & Target: HSF1[1]In Vitro: HSF1A protects cells from stress–induced apoptosis, binds TRiC subunits and inhibits TRiC activity without perturbation of ATP hydrolysis. Genetic inactivation or depletion of the TRiC complex results in human HSF1 activation and HSF1A inhibits the direct interaction between purified TRiC and HSF1 in vitro. Moreover, fluorescence anisotropy experiments using FITC coupled to HSF1A demonstrates that HSF1A–FITC binds to a purified Tcp1 subunit of TRiC with an affinity of approximately 600 nM. This is validated qualitatively via titration of purified Tcp1 into binding reactions containing 500 nM Biotin or HSF1A–Biotin [1]. Quantification bycounting the number of cell containing aggregates as a function of the total number of cells reveals that at HSF1A concentrations as low as 2 μM, a reduced number of aggregate–containing cells are observed. The fraction of cells containing aggregates continued to decrease in a dose–dependent manner such that pretreatment with 12 μM HSF1A resulta in ~20% of the cells exhibiting aggregates visible by fluorescence microscopy [2].In Vivo: HSF1A enhances HSF1 activity, stabilizes HSF1 expression and minimizes Doxorubicin (DOX)–induced cardiac damage. WKY rats are challenged with DOX (accumulated dose: 30 mg/kgw), and DOX combined with HSF1A (100 mg/kgw/day). Supplementation with HSF1A significantly elevates cardiac functions back to the levels of the control group. HSF1A has been shown to stimulate human HSF1 nuclear translocation, elevate protein chaperone expression and ameliorate protein misfolding and cell death in aneurodegenerative disease model. The echocardiographic results show that HSF1A also alleviates DOX–induced failures in cardiac function [3].PROTOCOL (Extracted from published papers and Only for reference)Kinase Assay:[1]Protein extracts are generated from mammalian, yeast and E. coli cultures using biotin–binding buffer (20 mM HEPES,5 mM MgCl 2, 1 mM EDTA, 100 mM KCl, 0.03% NP–40) supplemented with 1% Trition–X100 and protease inhibitors. Approximately 0.5mg of protein extract is incubated with 100 μM HSF1A–Biotin for 4 h at 4°C and HSF1A–Biotin associated proteins captured by with NeutrAvidin Agarose Resin. After washing in biotin binding buffer proteins are eluted using 50 μL biotin elution buffer (100 mM Tris,150 mM NaCl, 0.1 mM EDTA, 2 mM D–biotin), resolved on a 4–20% SDS–PAGE, and immunoblotted. For purified TRiC and Hsp70analyses, 5 nM protein is incubated in biotin–binding buffer+0.5% Triton X–100 with 100 μM biotin or 100 μM HSF1A–Biotin for 4 h at 4°C and captured with NeutrAvidin Resin. For NiNTA purified yeast Tcp1, different concentrations of Tcp1 0.5 μM, 1 mM, 2 mM, 3 mM and 4 mM in 25 mM Hepes pH 7.5, 150 mM NaCl are incubated with 0.5 μM Biotin or HSF1A–Biotin for 4 h at 4°C and captured with NeutrAvidin Resin [1].Cell Assay:[2]PC12 cells seeded into a 96–well plate (5×104 cells/well) are treated with increasing concentrations of HSF1A (2, 4, 8 andProduct Name:HSF1A Cat. No.:HY-103000CAS No.:1196723-93-9Molecular Formula:C21H19N3O2S2Molecular Weight:409.52Target:HSP Pathway:Cell Cycle/DNA Damage; Metabolic Enzyme/Protease Solubility:DMSO: ≥ 150 mg/mL12 μM) for 15 h, at which time httQ74–GFP expression is stimulated by incubation in the presence of 1 μg/mL Doxycycline for 5 d. Cell viability is assessed via the XTT viability assay[2].Animal Administration:[3]Rat[3]Ten–week–old Wistar Kyoto rats (WKY) are used. The rats are housed at a constant temperature (22°C) on a 12–h light/dark cycle with food and tap water. The animals are arranged into three groups: WKY rats (the control group), DOX rats and DOX rats treated with HSF1A. Each group contain five animals. The DOX group is injected with DOX (5 mg/kg) for 6 consecutive weeks intraperitoneal injection to achieve a cumulative dose of 30 mg/kg, which has been well documented to achieve cardiotoxicity. The small molecular HSF1 activator HSF1A (100 mg/kg/day) is injected intraperitoneally.References:[1]. Neef DW, et al. A direct regulatory interaction between chaperonin TRiC and stress–responsive transcription factor HSF1. Cell Rep. 2014 Nov 6;9(3):955–66.[2]. Neef DW, et al. Modulation of heat shock transcription factor 1 as a therapeutic target for small molecule intervention in neurodegenerative disease. PLoS Biol. 2010 Jan 19;8(1):e1000291.[3]. Huang CY, et al. Doxorubicin attenuates CHIP–guarded HSF1 nuclear translocation and protein stability to trigger IGF–IIR–dependent cardiomyocyte death. Cell Death Dis. 2016 Nov 3;7(11):e2455.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。
SAS-1
Hirsch Teil1. What are chemical sensors?- Definition !!!2. Selectivity- Definition- Equilibrium based selectivity: free energy, dielectric constant and distance,- Kinetic based selectivity: steady-state regime3. Recognition Methods- Ion recognition: recognition-electric charge, selectivity-size,transduction-potentiometric, optical methodse.g. PH electrode ----> part 3- Recognition by affinity interactions: reversible, non-covalent bonds-ionic bonds, hydrogen bonds, van der Waals interaction => result in a molecular assiciation complex; also respect to shape and chemical reactivity; indicated by stability constant (very stable)- antibody - antigen interaction => immunochemical reactionantibody: glycoprotein produced by immune system to identify and neutralizepathogen microorganisms.antigen: the part of the pathogen that reactions with the antibody.use specific antibody receptor => identify pathogenuse antigen receptor => identify antibody (the detection of infection byparticular pathogen)- lectin proteins recognize caborhydrates (agglutinins, hemagglutinin)carbohydrate-binding modules link to the catalytic part of glycosidehydrolases => result in degradation of cell wall, storage of polysaccharide- A Molecularly Imprinted Polymer (MIP) is a polymer that has been processed usingthe molecular imprinting technique which leaves cavities in polymer matrix withaffinity to a chosen "template" molecule.In chemistry, molecular imprinting is a technique to create template-shaped cavities in polymer matrices with memory of the template molecules to be used in molecular recognition.-Nucleic acid aptamers are nucleic acid species that have been engineered throughrepeated rounds of in vitro selection to bind to various molecular targets such assmall molecules, proteins, nucleic acids, and even cells, tissues and organisms.Aptamers are useful in biotechnological and therapeutic a pplications as they offer molecular recognition properties that rival that of the commonly used bimolecular antibodies.- Recognition by nucleic acids: hydrogen bonds between two distinct pairs of nucleobases => two complementary nucleic acids form a double strand association complex => called hybridizationnucleic acid sensors: short single strand NA as receptor to recognize a particular NA sequence in the analyte NA => detection of genetic anomalies and pathogen mircoorganism- Recognition by enzyme: dynamic processEnzyme: protein compound that function as catalysts in chemical reaction occurring in living system.- Recognition by cells and tissues: advantages of enzyme incorporated in biological materials => in their natural environmentsee part 3, Wegener - Recognition by gases and vapors: based on sorption at solid material => surface-adsorption, inner-absorption; purely physical phenomenon or chemical reaction.4. Transduction MetohdosChemical transduction: monitoring the change of chemical composition of the sensing element in response to the recognition process. => change in concentration/amount is measured => detect primary product -> secondary product or coreagent -> labeling productLABEL can be a simple molecular species or nanoparticals that can be detected by available physiochemical methods => enzyme, fluorescent dyes, luminescent dyes, electroactive compoundsPhysical transduction: a specific physical property of the sensing element that is affected by its interaction with the analyte is monitored. => mass, reflective index, dielectric properties, electrical resistivity => LABEL-FREE- Thermometric transductionRecognition of the analyte leads to change in temperature => only catalytical processes generate sufficient heat to the measurement => application: combustible gases react with O2 at the surface of a catalyst.- Transduction based on mechanical effectsRecognition leads to change in mass of the sensing element => monitored by mass tranducer based on quartz crystal microbalance (QCM)----------------------------------------------------------------------------------------------------------------- QCM, correct name: Thickness shear modePiezoelectric effect:generation of electrical charges on the surface of a solid by strain, pressure or torsion (mechanical deformation of solid) =>electricity resulting from pressureI nverse piezoelectric effect:application of charges to surfaces of piezoelectricsolid generates mechanical deformation (elongation, contraction, torsion)QCM is based on Inverse piezoelectric effect!# AT cut => 35`15`=> minimum temperature coefficient at 50~70 CIt makes the AT-cut well suited to applications requiring high degree of frequency stability over wide temperature ranges.## Electrodes are applied on both sides, and AC voltage applied.DC cannot flow across the crystal because it consists of an insulator material;however the crystal somewhat behaves as capacitor and allow an AC current to f low along the left-hand loop.AC voltage applied => leads to shear oscillation of crystal => when the voltage frequency matches the intrinsic vibration frequency of the crystal => the vibration amplitude is at maximal => the resonant => resonant frequency (f0) => depend on crystal thickness (e.g. d q= 330 um, f0= 5MHZ), density and elasticity of piezoelectric material### AT-cut resonator: thickness: ~0.2 mm, diameter of the active area: 5~20 mm #### Deposition of a homogenous mass film (a rigid overlay)Sauerbrey equation:Cf indicate sensitivity of QCMcondition of this equation: rigid deposited mass; △m<2% of crystal mass;operated in vacuum or in gaseous atmopphereIn liquid: the liquid breaks the vibration by friction => lessen f0Thickness of the layer must be greater than the wave decay lengththat is of 250 nm of 5 MHz resonator at water. ----> part 2!!!##### QCM in practice => see p.41----------------------------------------------------------------------------------------------------------------- - Resistive and capacitive transductionRecognition leads to changes in the electrical property of this materialResistive transduction: gases interact with MOS => change in electrical resistivity Capactive transduction => dielectric constant- Electrochemical transductionsee part 2, Matysik - Optical transductionOptical transduction can be based on light emission or light absorption, also by physical quantity (reflective index) and light scattering.5. Sensor Configuration and Fabrication- Lateral flow assayA typical test strip consists of the following components:1. Sample pad – an absorbent pad onto which the test sample is applied2. Conjugate pad –this contains antibodies specific to the target analyte;conjugated to coloured particles (e.g. gold nanoparticles)3. Reaction membrane –typically a hydrophobic nitrocellulose or celluloseacetate membrane onto which anti-target analyte antibodies are immobilized in a line across the membrane as a capture zone or test line, and a control zonecontaining antibodies specific for the conjugate antibodies.4. Wicking pad –a further absorbent pad designed to draw the sample acrossthe reaction membrane by capillary action and collect it.Double antibody sandwich assays: the sample migrates from the sample pad through the conjugate pad where any target analyte present will bind to the c onjugate.=> The sample then continues to migrate across the membrane until it reaches the test line where the target or conjugate complex will bind to the immobilized antibodies producing a visible line on the membrane. => The sample then migrates further along the strip until it reaches the control line, where excess conjugate will bind and producea second visible line on the membrane.This control line indicates that the sample has migrated across the membrane as intended. Two clear lines on the membrane is a positive result. A single line in the control zone is a negative result. Double antibody sandwich assays are most suitable for larger analytes, such as bacterial pathogens and viruses, with multiple antigenic sites. 6. Methods and Material in Sensor Preparation- Immobilization at solid surface => integration of a transducer with the receptor Physical adsorption at a solid supportNon covalent immobilization at solid surface => hydrophobic interaction, hydrogen bonding, electrostatic attraction; monolayer; no restrict access; not stable; Langmuir isotherm -> equilibrium interactionSupport material: silica, cellulose acetate, PVCCovalent bonding to the solid supportCovalent conjugation => stable, covalent bond, time consuming, expensiveCommon reactive group: -OH, -NH2, -C=O, -SH- Carboxylic acid with DCC- Glutaraldehyde reacts with the a.a. of lysine in protein => widely used Support: porous material => high specific area, high density of immobilized compounds => hydrogel: immobilized by entrapment/covalent corsslink - Natural polymers: Cellulose, Dextran- Synthetic polymers: Polystyrene- Active polymers: Epoxide (without preliminary activation) -->DNA array !!!- Inactive Polymers: Vicinal hydroxyls actived by CNBr- Inorganic support: Silica, AL2O3, TiO2 => stable at extreme PH- Metal support: noble metals, thiols on golds --> self assembled monolayers!Affinity reaction: avidin-biotin !!!Thin molecular layers: one or several molecular layers in solid support - Self-assembly of amphiphilic compounds: preparation of liposome andmicelles; liposome can be used of entrapment of molecular- Bilipid layer membranes: Langmuir-Blodgett technique- Layer by Layer assembly- Sol-Gel chemistry methods: silica gel => -O-Si-O-- Hydrogels: Xerogel, aerogel- Conducting polymers: Polyacetylene, polyaniline --> gas senor based on CP (----> part 3 !!!); also as entrapment matrix for biological receptors- Mesoporous materials: porous materials with pore (diameter: 2-50 nm,close to protein) => enzyme immobilization by entrapment (crosslinking withglutaraldehyde)- Deposition of polymers onto solid surfaces: dip coating, drop coating, spin coating ----> part 2 !!!Perm-selective memberanes: Nafin ----> Clark oxygen electrode Support-free crosslinkingEntrapment in a polymer networkEncapsulation7. Microfabrication Methodes- Spot Arraying: Contact-based & Noncontact-based; DNA microarray !!!!!Pros & Cons- Thick-film Technology: screen-printing technique (5-50 um thick layer)- Thin-film Technology: Photolithography (2 um)- Softlithography ----> experiment !!!!- Microcontact printing ----> experiment !!!!8. Optical Sensors- Electromagnetic RadiationOptical sensor => interaction of electromagnetic radiation with sensor layer - frequency; wavelength; photon energy (definition)- Structure: integration with wavelength-selection (optical filters) device and light sources (lasers), light detectors (phototransistors)- Optical Waveguides- Optical FibersOptical fibers' structuretotal internal reflection => evanescent wave- Spectrochemical Transduction MethodsSpectrochemical method analysis => light absorption or emission by sample => optical label performs absorption or emission (organic dye or metal complexes) - Light absorption: absorbance => concentration; sensitivity => thickness, absorpyivity, absorptivity => wavelength- Diffuse reflectance spectrometry: refelctance => concentration; suitable forsolid in near IR- Luminescence: Fluorescence spectromerty => fluorophore (label, organic dye or metal complexes, luminescent nanparticle ); steady-statefluorescence measurement, Time-resolved fluormetry; fluorescencequenching; resonance energy transfer (FRET); chemical- andbioluminescence => luminol; electrochemicaluminescence; Ramanspetrometry- Surface Plasmon Resonance Spectroscopy (SPR)。
超高效液相色谱-串联质谱法测定人血浆中精氨酸及衍生物含量
超高效液相色谱-串联质谱法测定人血浆中精氨酸及衍生物含量田晔;江骥;胡蓓;薛金萍;王洪允【摘要】建立了超高效液相色谱-串联质谱(UPLC-MS/MS)法同时测定使用艾普拉唑后人血浆中二甲基精氨酸(ADMA)、对称二甲基精氨酸(SDMA)、单甲基精氨酸(NMMA)、瓜氨酸(Cit)和L-精氨酸(L-Arg)的浓度.采用HILIC亲水相互作用色谱和非衍生化的蛋白沉淀法进行分离分析,色谱柱选取Waters Atlantic HILIC柱(2.1 mm×50 mm×3μm),流动相由乙腈(含0.5％乙酸和0.025％三氟乙酸)-水(含0.5％乙酸和0.025％三氟乙酸)(85:15,v/V)组成,流速0.25 mL/min.采用多反应离子监测(MRM)模式,以电喷雾离子源(ESI)正离子方式检测.结果显示,ADMA、SDMA、NMMA、L-Arg和Cit的线性关系良好,相关系数r均大于0.994 0;ADMA、SDMA和NMMA的线性范围为0.1～5 mmol/L,L-Arg和Cit的线性范围为10～250 mmol/L;5种氨基酸的日内、日间精密度均小于15％,准确度在85％～115％之间.该方法快速、简便、灵敏,可为相关疾病的临床诊断提供一种高效的检测手段.【期刊名称】《质谱学报》【年(卷),期】2016(037)005【总页数】7页(P446-452)【关键词】超高效液相色谱-串联质谱(UPLC-MS/MS);艾普拉唑;蛋白沉淀法;亲水性色谱【作者】田晔;江骥;胡蓓;薛金萍;王洪允【作者单位】福州大学化学学院,福建省功能材料工程研究中心,福建省光动力治疗药物与诊疗工程技术研究中心,福建福州350108;中国医学科学院北京协和医院临床药理中心,北京100730;中国医学科学院北京协和医院临床药理中心,北京100730;中国医学科学院北京协和医院临床药理中心,北京100730;福州大学化学学院,福建省功能材料工程研究中心,福建省光动力治疗药物与诊疗工程技术研究中心,福建福州350108;中国医学科学院北京协和医院临床药理中心,北京100730【正文语种】中文【中图分类】O657.63一氧化氮是人体重要的信使分子，L-精氨酸(L-Arg)在一氧化氮全酶(NOS)的催化下，产生一氧化氮(NO)和瓜氨酸(Cit)[1-2]。
EL-102_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 :EL-102Catalog No. :HY-16187CAS No. :1233948-61-21.2 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:EL 102; EL102Formula:C19H16N2O3S2Molecular Weight:384.47CAS No. :1233948-61-24. 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。
一种盐酸溴己新片溶出度的检测方法
一种盐酸溴己新片溶出度的检测方法在制药工业中，溶出度（dissolution）是一种重要的参数，用来评估固体药物在溶液中的释放速度。
而对于盐酸溴己新片这种常用的药物成分，其溶出度的检测更是至关重要。
为了确保盐酸溴己新片的治疗效果，制药公司需要对其溶出度进行精确测定。
然而，由于盐酸溴己新片的特性，传统的溶出度检测方法往往存在一些局限性。
研究人员不断探索新的检测方法，以更准确、高效地评估盐酸溴己新片的溶出度。
一种最新的盐酸溴己新片溶出度检测方法基于高效液相色谱-质谱联用技术（HPLC-MS），该方法在传统的溶出度检测方法的基础上进行了革新和优化。
通过这种方法，不仅可以准确地分析盐酸溴己新片在不同时间点的溶出度曲线，还可以同时检测其代谢产物和降解物，从而更全面地了解盐酸溴己新片在溶液中的行为。
该方法利用高效液相色谱技术，可以将盐酸溴己新片及其代谢产物和降解物进行有效分离，从而确保溶出度检测的准确性。
随后，利用质谱技术对分离得到的化合物进行准确的定性和定量分析，进一步提高了检测结果的可信度。
值得一提的是，该方法还可以与自动取样系统结合，实现对多个样品的快速、连续检测，大大提高了检测效率，降低了人工操作的影响。
该方法还可以在一定程度上降低了溶出度检测的成本，适用于大规模的生产和质量控制过程。
通过对盐酸溴己新片溶出度的全面监测，制药公司可以更好地了解药物在不同条件下的释放情况，优化配方和工艺参数，从而提高产品的稳定性和疗效一致性。
这种高效的检测方法也为新药物的研发和监管提供了可靠的技术支持。
盐酸溴己新片溶出度的检测方法是制药工业中至关重要的一环。
高效液相色谱-质谱联用技术作为一种创新的检测方法，为盐酸溴己新片的溶出度检测提供了全新的思路和解决方案。
相信随着科学技术的不断进步，我们会看到更多更先进的方法应用于药物溶出度的监测，为制药行业的发展注入新的活力。
以上是个人对盐酸溴己新片溶出度检测方法的一些观点和理解，希望对你有所帮助。
硫酸沙丁胺醇雾化吸入溶液冻融稳定性研究
2019年第9期广东化工第46卷总第395期·97·硫酸沙丁胺醇雾化吸入溶液冻融稳定性研究毛毅斌1，徐欣1，刘哲鹏2，孙涛2(1．上海信谊金朱药业有限公司，上海201500；2．上海理工大学，上海200093)Study on Freeze-thaw Stability of Salbutamol Sulfate InhalationMao Yibin1,Xu Xin1,Liu Zhepeng2,Sun Tao2(1.Shanghai Xinyi Jinzhu Pharmaceutical Co.;Ltd.,Shanghai201500；2.University of Shanghai for Science and Technology,Shanghai200093,China)Abstract:In this experiment,the freeze-thaw stability of salbutamol sulfate aerosol inhalation solution was investigated by repeated freeze-thaw method.The salbutamol sulfate atomized inhalation solution was placed in a refrigerator(-10℃to-20℃)for two days,taken out and placed in a40℃stable box for two days, taken out three times,placed at room temperature,and observed for appearance and Detect its content and related substances.The results showed that the appearance traits,pH,content and related substances were all in compliance with the standard,and the solution stability was good.Keywords:Salbutamol sulfate；freeze-thaw；content；related substances硫酸沙丁胺醇雾化吸入液是一种临床上应用广泛的β2肾上腺受体激动药，为无色澄明液体，可以预防及治疗支气管哮喘，治疗伴有可逆性支气管阻塞[1]。
QPCR及QRT-PCR系列产品
Invitrogen的ICFC系列产品促销1．QPCR及QRT-PCR系列产品Invitrogen公司专门为中国客户提供的定量PCR试剂盒，结合了 UDG 防止残余污染技术和SYBR® Green I 荧光染料（存在于SYBR® Green I荧光定量PCR试剂盒中），在美国接受了严格的质量监控，可提供极高灵敏度的目的序列定量检测，线性剂量低，反应浓度范围很大。
qPCR Supermix-- 即用型反应剂，专为高特异性、实时定量DNA扩增设计UDG-- 防止携带污染物，减少克隆片段假阳性结果ROX参考染料-- 适用ABI仪器的校正染料产品信息活动时间：即日起至2009年4月30日2．Gibco南美胎牛血清即日起凡优惠价¥1780购买Gibco胎牛血清500ml（目录号:C2027050）即可获赠送价值¥250现金抵用券。
您可以凭现金抵用券在英韦创津公司购买任何商品，此券有效期至2009年5月31日。
产品信息活动时间：即日起至2009年4月30日独特的采集方式：GIBCO采用无菌心脏穿刺的方式采血原装直送，避免污染：原产地采集、加工、检测、包装。
完善的质控：采集、处理、检测、运输等环节都有文件和证书。
3．Invitrogen TA Cloning克隆产品专门用于克隆Taq聚合酶扩增的PCR产物。
采用pCR载体，能产生80%以上的重组产物，90%以上重组产物都包含插入片段。
产品信息活动时间：即日起至2009年5月31日附：pCR载体优点及图谱：3’-T突出端可直接连接Taq扩增的PCR产物可选择T7或T7和Sp6启动子进行体外RNA转录和测序侧向EcoRⅠ位点的通用多接头位点方便了插入片段的切离可以选择卡那霉素或氨苄青霉素进行筛选非常简便的蓝/白克隆筛选具有M13正向和反向引物位点，方便测序4．GIBCO液体培养基系列产品创立近50年的历史，品质优秀，产品种类丰富；为了中国用户利益，特建立国内生产线；所有产品，从原材料到生产全部按照GIBCO质量标准进行，每批均送抵美国公司总部质检合格后，才在国内销售。
气相色谱法测定盐酸美金刚原料药中有机溶剂残留量
精 密 量 取 ２ 项 下 的 对 照 储 备 液 ． ２
１ ，．，．， ．，．，． ，分 别 置 于 ｌｍｌ 瓶 中 ， ． ２０ ４０ ５０ ６０８０ ０ ｍｌ Ｏ 量 另 分 别精 密量 取 内标储 备 液 １ ｍ 置 上 述 量 瓶 中 ， ． ｌ ０
分别精密量取对照储备液 ５ ｍ 和内标储备液 ． ｌ ０ １ ｍ 置 １ｍｌ 瓶 中 ， 溶 剂 稀 释 至 刻 度 ， 匀 即 ． ｌ ０ ０ 量 加 摇
色谱柱 ：Ｂ ５毛细管色谱柱（０ ５ｍ Ｄ一 ３ｍ Ｘ ． ｍ× ０３
１ｕ ５ ． ｍ）％苯基 一 ５ ５ ９ ％Ｚ． 聚硅 氧烷 ； 甲基 检测 器 ： 火 氢
焰离 子 化检 测 器 （Ｉ ， 测 温度 ：８ Ｔ ； 样 口温 ＦＤ）检 ２ ０ ；进 度 ：３ ℃ ； 温 ：０ ２０ 柱 ５ ％保 持 １ｍｉ， 后 以 ３ ℃／ｉ ２ ｎ然 ０ ｍｎ 升 温 至 ２０Ｃ， ３ ￣ 至少 保 持 ｌ 钟 ； 气 ： 纯 氮 ， ２分 载 高 流 速 １ ｍｌ ｎ 分流 比 ：０１直 接进 样 ， 样量 ： ｌ ． ／ ； ０ ｍｉ １：； 进 １ 。 在 上 述 色谱 条 件 下 ， 剂 乙醇 、 溶 乙腈 、 乙醚 、 二 氯 甲 烷 的 保 留 时 间 分 别 为 ：． ７ ８８４ ９２０ ８０ 、． 、．３ 、 ８ ２ １． ６ｍｉ， 内 标 物 质 乙 酸 乙 酯 的 保 留 时 间 为 ０１ ｎ ６ １．７ｍｉ。 ３１６ ｎ 计算 结果 表 明上 述各 溶剂 分离 度均 大 于 ２０ 理论 塔板 数均 大于 １０ ０ ．， ０ ０ 。色谱 图见 图 ｌ 。
作者简介 ： 以兵（ ９ ４ ， ， 余 １７ 一）男 工程师 ， 主要从事药物分析 工作 。Ｅ ｍａ ：ｈ７ １０ Ｃ ｒ ｏ． ｍｅ － ｉ ｃｂ４ １ ２￣ａ ｏ ｏ ． ｌ ６ｈ ｅ ｎ
一种国产胃泌素释放肽前体化学发光免疫试剂的性能验证
一种国产胃泌素释放肽前体化学发光 免疫试剂的性能验证
欧赛英１，徐海伟１，陈秀发１，沙利烽１，梁 辰２，冯 杰２，薛 辉２，颜光涛２
（１．苏州长光华医生物试剂有限公司，江苏 苏州 ２１５１６３； ２．中国人民解放军总医院医学检验中心，北京 １００８５３）
ＴｈｅＰｅｒｆｏｒｍａｎｃｅＶｅｒｉｆｉｃａｔｉｏｎｏｆａＤｏｍｅｓｔｉｃＧａｓｔｒｉｎｒｅｌｅａｓｉｎｇ ＰｅｐｔｉｄｅｆｏｒＣｈｅｍｉｌｕｍｉｎｅｓｃｅｎｃｅＩｍｍｕｎｏｒｅａｇｅｎｔ
ＯＵ Ｓａｉｙｉｎｇ１，ＸＵ Ｈａｉｗｅｉ１，ＣＨＥＮ Ｘｉｕｆａ１，ＳＡ Ｌｉｆｅｎｇ１，ＬＩＡＮＧ Ｃｈｅｎ２， ＦＥＮＧ Ｊｉｅ２，ＸＵＥＨｕｉ２，ＹＡＮ Ｇｕａｎｇｔａｏ２
（１．ＳｕｚｈｏｕＣｈａｎｇｇｕａｎｇｈｕａＭｅｄｉｃａｌＲｅａｇｅｎｔＣｏ．ＬＴＤ，Ｓｕｚｈｏｕ２１５１６３，Ｃｈｉｎａ； ２．ＭｅｄｉｃａｌＬａｂｏｒａｔｏｒｙＣｅｎｔｅｒｏｆＰＬＡ ＧｅｎｅｒａｌＨｏｓｐｉｔａｌ，Ｂｅｉｊｉｎｇ１００８５３，Ｃｈｉｎａ）
Ａｂｓｔｒａｃｔ：ＯｂｊｅｃｔｉｖｅＰｒｏＧＲＰｉｓａｐｒｏｍｉｓｉｎｇｅｆｆｅｃｔｉｖｅｔｕｍｏｒｍａｒｋｅｒｉｎｄｉｓｃｒｉｍｉｎａｔｉｎｇＳＣＬＣｆｒｏｍ ＮＳＣＬＣａｎｄ ｏｔｈｅｒｂｅｎｉｇｎｌｕｎｇｄｉｓｅａｓｅｓ．ＰｒｏＧＲＰＣｈｅｍｉｌｕｍｉｎｅｓｃｅｎｔｉｍｍｕｎｏａｓｓａｙ（ＣＬＩＡ）ｗａｓｄｅｖｅｌｏｐｅｄａｎｄｍａｎｕｆａｃｔｕｒｅｄ ｂｙＨｙｂｉｏｍｅ．Ｔｈｅｍａｎｕｆａｃｔｕｒｅｒｄｅｃｌａｒｅｄｔｈｅｐｅｒｆｏｒｍａｎｃｅｐａｒａｍｅｔｅｒｓａｓｆｏｌｌｏｗｉｎｇ：ｔｈｅｐｒｅｃｉｓｉｏｎｏｆｔｈｅｒｅａｇｅｎｔ ｗａｓｌｅｓｓｔｈａｎ１０％，ｔｈｅｌｉｍｉｔｏｆｄｅｔｅｃｔｉｏｎｗａｓ５ｐｇ／ｍＬ，ｔｈｅｒｅｃｏｖｅｒｙｗａｓｂｅｔｗｅｅｎ ＜±１０％，ｔｈｅｒｅｆｅｒｅｎｃｅ ｒａｎｇｅｗａｓ＜６５ｐｇ／ｍＬ，ｔｈｅｌｉｎｅａｒｒａｎｇｅｗａｓ１５３０００ｐｇ／ｍＬ，ｔｈｅｓｅｒｕｍ ｗａｓｗｅｌｌｃｏｒｒｅｌａｔｅｄｗｉｔｈｐｌａｓｍａ，ａｎｄ ｔｈｅｓｅｒｕｍ ｓｔａｂｉｌｉｔｙｃｏｕｌｄｒｅａｃｈ９６ｈｏｕｒｓ，ａｎｄｔｈｅｃｏｒｒｅｌａｔｉｏｎｗｉｔｈＲｏｃｈｅｅｌｅｃｔｒｏｃｈｅｍｉｌｕｍｉｎｅｓｃｅｎｃｅｐｒｏＧＲＰ ｒｅａｇｅｎｔｗａｓｇｏｏｄ．Ｔｈｅｐｅｒｆｏｒｍａｎｃｅｏｆｔｈｅｒｅａｇｅｎｔｗａｓｖｅｒｉｆｉｅｄｉｎｔｈｉｓｓｔｕｄｙ．ＭｅｔｈｏｄｓＡｃｃｏｒｄｉｎｇｔｏｔｈｅＣＬＳＩ ａｎｄＣＡＰ，ｔｈｅｐｒｅｃｉｓｉｏｎ，ｌｉｍｉｔｏｆｑｕａｎｔｉｔａｔｉｏｎ，ｒｅｃｏｖｅｒｙｒａｔｅ，ｌｉｎｅａｒｒａｎｇｅ，ｒｅｆｅｒｅｎｃｅｉｎｔｅｒｖａｌ，ｓｅｒｕｍ ｐｌａｓｍａ ｃｏｎｓｉｓｔｅｎｃｙ，ｓｅｒｕｍ ｓｔａｂｉｌｉｔｙａｎｄｃｏｍｐｌｅｍｅｎｔｉｎｔｅｒｆｅｒｅｎｃｅｏｆｔｈｅｄｏｍｅｓｔｉｃｐｒｏＧＲＰａｓｓａｙａｎｄｉｔｓｓｕｐｐｏｒｔｉｎｇ ｉｎｓｔｒｕｍｅｎｔ，ＡＥ１８０ｄｅｔｅｃｔｉｏｎｓｙｓｔｅｍ，ｗｅｒｅｖｅｒｉｆｉｅｄ．１９９ｃａｓｅｓａｍｐｌｅｓｆｒｏｍ ｈｅａｌｔｈｙｃｏｎｔｒｏｌ，ｓｍａｌｌｃｅｌｌｌｕｎｇ ｃａｎｃｅｒ，ｎｏｎｓｍａｌｌｃｅｌｌｌｕｎｇｃａｎｃｅｒａｎｄｂｅｎｉｇｎｌｕｎｇｄｉｓｅａｓｅｐａｔｉｅｎｔｓ，ｗｅｒｅｄｅｔｅｃｔｅｄｉｎｐａｒａｌｌｅｌｗｉｔｈＲｏｃｈｅＥ６０１ ｓｙｓｔｅｍ ｔｏｃｏｍｐａｒｅｔｈｅｃｏｎｓｉｓｔｅｎｃｙｏｆｔｈｅｒｅｓｕｌｔｓｂｅｔｗｅｅｎｔｈｅｔｗｏｄｅｔｅｃｔｉｏｎｓｙｓｔｅｍｓ．ＲｅｓｕｌｔｓＴｈｅｎｅｗＰｒｏＧＲＰ
稳态荧光探针法测定SDS表面活性剂胶束聚集数
稳态荧光探针法测定SDS表面活性剂胶束聚集数
陈红梅
【期刊名称】《广东化工》
【年(卷),期】2009(36)8
【摘要】以芘作为荧光探针,十六烷基氯化吡啶(CPC)作为猝灭剂,根据芘的荧光强度之比随表面活性剂水溶液浓度的变化,测定十二烷基硫酸钠(SDS)的临界胶束浓度(cmc),测定值与文献值较一致.并用外推法得到SDS的胶束聚集数(n).文章提供了一种简单可行的实验方法了来计算和评价胶束的基本特性.
【总页数】2页(P219-220)
【作者】陈红梅
【作者单位】武汉工业学院,化学与环境工程系,湖北,武汉,430023
【正文语种】中文
【中图分类】O65
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3.稳态荧光探针法测定临界胶束聚集数 [J], 方云;刘雪锋;夏咏梅;杨扬;蔡琨;徐廷穆;赵宪英
4.稳态荧光探针法测定松香基季铵盐Gemini表面活性剂胶束聚集数 [J], 蒋福宾;
曾华辉;杨正业;李俊杰;宋宝玲
5.一类新的表面活性剂——长链烷基三苯基鏻——Ⅵ.稳态荧光猝灭法测定十二烷基三苯基溴化鏻胶束的平均簇集数 [J], 江云宝;许金钩;陈国珍
因版权原因，仅展示原文概要，查看原文内容请购买。
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)。
毛细管胶束电动色谱法分离测定中药半枝莲中的7种有效成分
毛细管胶束电动色谱法分离测定中药半枝莲中的7种有效成分米璇;朱若华【期刊名称】《色谱》【年(卷),期】2010(28)2【摘要】建立了毛细管胶束电动色谱同时分析检测中药半枝莲药材及其膏剂中黄芩素、柚皮素、汉黄芩素、野黄芩苷、芹菜素、木犀草素和原儿茶酸7种有效成分的方法.半枝莲样品中7种有效成分经甲醇超声提取.实验考察了运行缓冲溶液的pH值和浓度、添加剂、检测波长、分离电压和进样时间等重要参数对目标物分离的影响.得到的优化条件为:运行缓冲液50 mmol/L 硼砂-0.20 mol/L 硼酸溶液(pH 8.4),含8.5 mmol/L 十二烷基硫酸钠(SDS),分离电压25 kV,检测波长260 nm和335 nm.在此条件下,7种组分于12 min内达到基线分离.各组分在8×10~(-6)～3.2×10~(-4) mol/L 范围内呈良好的线性关系,相关系数(r~2)为 0.996 5～0.999 9;检出限为7.0×10~(-8)～2.0×10~(-6) mol/L;回收率均大于85% .该方法提取简便、准确可靠、重复性好、灵敏度高,可以用于中药半枝莲中7种有效成分的定量检测.【总页数】6页(P209-214)【作者】米璇;朱若华【作者单位】首都师范大学化学系,北京,100048;首都师范大学化学系,北京,100048【正文语种】中文【中图分类】O658【相关文献】1.混合胶束-电动毛细管色谱法分离测定性激素 [J], 李晓静;徐翔;李永库2.毛细管胶束电动色谱法用于石韦药材中绿原酸、槲皮素和山奈酚的分离测定 [J], 宋子旺;刘远环;张兰3.在线扫集-胶束电动毛细管色谱法对活血通脉片中阿魏酸与原儿茶醛的分离测定[J], 李利军;胡大春;郝学超;吴启涛;李彦青4.胶束电动毛细管色谱法测定穿心莲中穿心莲内酯和脱水穿心莲内酯 [J], 李琦;胡广林;徐晓琴;庄峙厦;王小如5.在线扫集-胶束毛细管电动色谱法分离测定急支糖浆中阿魏酸、原儿茶醛和原儿茶酸 [J], 李利军;张瑞瑞;孙科;杨兰兰;崔福海;罗应;李彦青因版权原因，仅展示原文概要，查看原文内容请购买。
GC测定盐酸普拉克索中三乙胺残留量
盐 酸 普拉 克索 (pramipexole hydrochloride) 是 一种非麦角类衍生物，主要用于治疗帕金森氏综 合症， 其化学名称为(s)-2-氨基-4,5,6,7-四氢-6-丙基 氨苯噻唑二盐酸盐一水合物，分子式为 C10H17N3S·2HCl·H2O，分子量为 284.25。它可高度 选择性地作用于多巴胺 D2 受体， 对多巴胺的神经 有保护作用，它可单独使用或与左旋多巴联合用 药治疗早期帕金森，对不宁腿综合症也有效
钠溶液，10%，20%的氢氧化钠溶液，结果表明三 乙胺的检测灵敏度随着碱性的增强而增加，重复 性、回收率随着碱度的增强而增强。当采用 20% 的氢氧化钠溶液作为溶剂，虽然样品因为其中的 盐酸被中和掉而析出，但是在加入溶剂充分振摇 后，重复性、回收率均良好，因此选用 20%的氢 氧化钠溶液作为溶剂。这也为盐酸、醋酸等酸性 盐类药物中三乙胺的残留检测提供了一种思路。 3.2 顶空平衡条件的选择 三乙胺的沸点为 89.5 ℃，顶空平衡温度的选 择，需兼顾各种溶剂的沸点与性质，考虑到顶空 平衡温度过高 (>90 ℃) 会使溶剂膨胀导致压力升 高，引起顶空瓶的耐压和仪器气密性等问题[4]，因 此参照欧洲药典相关规定选择温度 80 ℃作为顶空 平衡温度。本实验以平衡温度为 80 ℃时，平衡时 间分别为 20，30，40，50 min 时的色谱响应值(面 积 ) 进行实验，发现其响应值逐渐增加，在平衡 30 min 与平衡 40 min 的响应基本一致，说明在 30 min 时，三乙胺在气液两相间达到平衡，故本 实验选择 30 min 作为顶空平衡时间。 3.3 色谱柱的选择 三乙胺属强极性物质，考察了 DB-624、DBFFAP、 HP-5 等多根毛细管色谱柱， 均发现严重拖尾 现象， 最终选择 100%二甲基聚硅氧烷为固定液的较 粗口径 DB-1 毛细管柱(30 m×0.53 mm，1.0 μm)， 峰型较好，理论板数最高，为 15 234。