Key Laboratory of Drug Quality Control and Pharmacovigilance (China Pharmaceutical University), Ministry of Education, Nanjing 210009, China.
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。
