摘要
目的采用LC-MS/MS测定人血浆中的氨氯地平。方法血浆样品经氢氧化钠碱化,乙酸乙酯萃取后进行分析。使用Gmini C18 110A(50 mm×3 mm,5μm)色谱柱,流动相为甲醇-水-甲酸(55:45:0.025),流速0.2 ml·min^-1,通过电喷雾离子化四极串联质谱,以多反应离子方式检测。氨氯地平m/z409.4→237.9和莫沙比利m/z422.1→198.0。结果线性范围为0.0313~20 ng·ml^-1,最低定量限为0.0313 ng·ml^-1,萃取回收率为74.4%~83.1%,方法回收率为96.1%~108.7%,日内和日间RSD均〈8%。结论所用方法快速、简便、灵敏度高,适用于人血浆中药物浓度的测定及药物动力学和生物利用度的研究。
OBJECTIVE To develop an LC - MS/MS method for determination of Amlodipine in human plasma. METHODS Amlodipine and internal standard, mosapride, extracted from plasma with accetate after being alkalized by NaOH, and then separated on a Gmini C18 110A column (50 mm × 3.00 mm, 5 μm). The mobile phase consisted of methanol -water- formic acid (55 : 45 : 0. 025 ) , and the flow rate was 0.2 ml· min^- 1. The sample were subsequently analyzed by mass spectrometry with an ESI source and then quantified by multiple reaction monitoring ( MRM ). The precursor - product ion combinations of m/z 409.4 →237.9 and m/z 422.1→198.0 was used to quantify Amlodipine and internal standard, respectively. RESULTS The standard curve was linear in the range of 0.0313 - 20 ng· ml^ - 1. The limit of quantification was 0.0313 ng· ml^ - 1. The extraction recovery of Amlodipine were 74.4% - 83, 1% and methodology recovery were 96.1% - 108.7% and the within - day and between - day RSDs were less than 8%. CONCLUSION The method is proved to be suitable for determination of Amlodipine in human plasma after oral administration of low dosage, which offers advantage of much high sensitivity than the previously reported methods.
出处
《华西药学杂志》
CAS
CSCD
北大核心
2009年第5期512-514,共3页
West China Journal of Pharmaceutical Sciences