一种用于同时测定人血浆中四种 H2 拮抗剂的单 LC-串联质谱法。
A single LC-tandem mass spectrometry method for the simultaneous determination of four H2 antagonists in human plasma.
机构信息
Key Laboratory of Drug Quality Control and Pharmacovigilance (China Pharmaceutical University), Ministry of Education, Nanjing 210009, China.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2009 Dec 1;877(31):3953-9. doi: 10.1016/j.jchromb.2009.10.003. Epub 2009 Oct 8.
A sensitive and universal LC-MS/MS method for the simultaneous determination of famotidine, cimetidine, ranitidine and lafutidine in human plasma was presented. This is the first single LC-MS/MS method reported for the simultaneous analysis of these four H(2) antagonists in human plasma. Following liquid-liquid extraction with ethyl acetate, the separation was performed on an Agilent Zorbax SB-CN (150 mm x 2.1mm I.D., 5 microm) column using a mobile phase consisted of methanol:20 mM ammonium acetate (55:45, v/v). The total run time was 7 min per sample. Quantification was performed by electrospray ionization-triple quadrupole mass spectrometry by selected reaction monitoring (SRM) detection in the positive mode. All calibration curves showed good linear regression (r(2)>0.99) from 0.5 to 1000 ng/mL for famotidine and lafutidine, and 5-20,000 ng/mL for cimetidine and ranitidine. The method showed good precision and accuracy with overall intra- and inter-day variations of 1.37-9.29% and 3.51-9.40%, respectively. The assay was successfully applied to a bioequivalence study using ranitidine as the model compound.
一种灵敏且通用的 LC-MS/MS 法，用于同时测定人血浆中的法莫替丁、西咪替丁、雷尼替丁和拉呋替丁。这是首次报道的用于同时分析人血浆中这四种 H2 拮抗剂的单一 LC-MS/MS 方法。采用乙酸乙酯进行液液萃取后，在 Agilent Zorbax SB-CN（150mmx2.1mmID，5μm）柱上，以甲醇：20mM 乙酸铵（55：45，v/v）为流动相进行分离。每个样品的总运行时间为 7 分钟。通过电喷雾电离-三重四极杆质谱法，以正模式下的选择反应监测（SRM）检测进行定量。所有校准曲线均显示出良好的线性回归（r²>0.99），法莫替丁和拉呋替丁的线性范围为 0.5-1000ng/mL，西咪替丁和雷尼替丁的线性范围为 5-20000ng/mL。该方法显示出良好的精密度和准确度，日内和日间总变异分别为 1.37-9.29%和 3.51-9.40%。该测定法成功应用于以雷尼替丁为模型化合物的生物等效性研究。
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