摘要
目的:建立高效液相色谱-串联质谱法(HPLC-MS/MS)测定人血浆中莫沙必利含量及其代谢物(M1)的相对含量。方法:采用Phenomenex Gemini C18色谱柱(50 mm×3.0 mm,3μm),流动相为甲醇-0.04%甲酸(58∶42)。血浆样品在碱性条件下用乙酸乙酯提取浓集后进样,以西沙必利为内标,MRM模式检测。莫沙必利,M1和内标检测离子对的m/z分别为422.1/198.0,314.3/198.1和466.2/184.0。结果:莫沙必利在0.25~128μg.L-1范围内线性关系良好(r=0.9999),最低定量限为0.25μg.L-1,方法回收率为99.8%~103.5%,批内?批间RSD分别小于5.2%及6.4%。结论:本法具有快速、灵敏、准确等特点,适用于莫沙必利血药浓度测定及药代动力学研究和血浆中莫沙必利代谢物M1的测定。
Objective: To establish a HPLC-MS/MS method for the determination of mosapride(MS) and its metabolite(M1) in human plasma . Methods: Phenomenex Gemini C18 column (50mm×3.0 mm,3 μm) was used. The mobile phase was methanol-0.04% formic acid (58 : 42). The alkalinized sample was extracted with acetic ether and the content of drug was determined by HPLC-MS/MS using electrospray ionization. MS, M1 and Cisapride(IS) were detected on multiple reaction monitoring(MRM) mode by the transitions from the precursor to the production (m/z: 422.1/198.0, 314.2/198.1 and 466.2/184.0). Results: For MS, calibration curve was linear in range from 0.25 to 128μg·L^-1 (r = 0.9999), the limit of quantitation in plasma was 0.25μg·^L-1, the method recovery was 99.8 %-103.5 %, the RSD of inter- and intra-day precision were less than 5.2 % and 6.4 %, respectively. Conclution: This method is found to be rapid, sensitive and accurate for determination of MS and its metabolite in human plasma.
出处
《药物分析杂志》
CAS
CSCD
北大核心
2009年第11期1842-1845,共4页
Chinese Journal of Pharmaceutical Analysis