摘要
目的:应用液相色谱-三重四极杆质谱分析苯唑西林钠的碱性降解物。方法:采用C18色谱柱(250 mm×4.6 mm,5μm);流动相:0.01 mol.L-1醋酸铵溶液(醋酸调pH至5.0)-乙腈(75∶25);流速:1.0 mL.m in-1;检测波长:225 nm;柱温:30℃;液相出口分流20%进入四极杆质谱,以电喷雾电离源正离子模式(ESI+)进行质谱数据采集。结果:得到苯唑西林钠碱性降解物液相色谱图以及液相色谱峰对应的一级质谱图。对谱图进行分析归纳,推测苯唑西林钠碱性降解物中4个主要组分分别为苯唑西林的青霉噻唑酸及其异构体、苯唑西林的脱羧青霉噻唑酸以及6-APA与苯甲异唑酰氯的缔合物。结论:本方法灵敏、可靠、快速,为杂质控制和工艺改进提供了有力帮助,对苯唑西林钠质量的提高及杂质含量控制指标的制订具有重要的指导意义。
Objective：To analyze impurities degraded by alkali in oxacillin sodium by using liquid chromatogramand and triple quadropole mass spectrometry.Methods：Using C18 column（250 mm×4.6 mm,5 μm）;0.01 mol·L-1 ammonium acetate（pH 5.0）-acetonitrile（75∶25） as mobile phase,temperature：30 ℃,the flow rate：1.0 mL·min-1,detection wavelength：225 nm;20% of the liquid exit come into the quadropole mass spectrometry and collect the mass spectral date about ESI＋.Results：The penicilloic acid of oxacillin and its isomer,decarboxylation penicilloic acid of oxacillin,the associated compound of phenacyl 6-aminopenicillinate and 5-methyl-3-phenylisoxazole-4-carbonyl chloride,as impurities degraded by alkali in oxacillin sodium have been determined by the liquid chromatogram and its first order mass spectrum.Conclusion：The method is sensitive,rapid and credible in production and quality control of oxacillin sodium.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2011年第6期1102-1105,共4页
Chinese Journal of Pharmaceutical Analysis
关键词
苯唑西林钠
降解物
杂质
青霉噻唑酸
异构体
电喷雾离子化质谱
分析
oxacillin sodium
degradation products
impurities
penicilloicacid
isomer
electrospray ionization mass spectrometry
analysis
