高效液相色谱-质谱法测定人血浆中左卡尼汀的浓度  

Determination of Levocarnitine in Human Plasma by HPLC-MS/ESI

作　　者：程钢[1,2] 朱荣华[2] 李明铁[3] 彭文兴[1] 

机构地区：[1]中南大学湘雅二医院临床药学研究室,长沙410011 [2]湖南省常德市第一人民医院,湖南常德415003 [3]桂林医学院2005级实习生,广西桂林541004

出　　处：《中国药学杂志》2009年第20期1571-1574,共4页Chinese Pharmaceutical Journal

摘　　要：目的建立人血浆中左卡尼汀浓度的高效液相色谱一质谱（HPLC．MS）测定法。方法以米屈肼作为内标，血浆样品经蛋白沉淀法处理，用氰基色谱柱（UltimateXB—CN，4．6mm×250mm，5μm）进行分离，以乙腈．30mmol，L-1醋酸铵水溶液（含0．8％甲酸1（80：20）为流动相，柱温40℃，流速1．0mL·min-1，柱后分流比为4：1，HPLC—MS／ESI＋法选择性监测准分子离子峰[M＋H]＋（左卡尼汀：m／z=162．1，Is：m／z=147．1）。结果左卡尼汀及内标米屈肼在氰基柱上保留较好，分离完全，左卡尼汀在0．4～12．8mg·L-1内线性关系良好，r=0．9994，平均萃取回收率大于80％，方法回收率大于92％，小于114％，日内日间RSD均小于12％。结论本方法简便快速、灵敏准确，适用于人血浆中左卡尼汀临床治疗监测和药物研究的需要。OBJECTIVE To establish a HPLC-MS method for the determination ofmildronate in human plasma. METHODS The analytes in plasma were extracted by protein precipitation using acetonitrile. The extracts were analyzed by a high performance liquid chromatography coupled with eleetrospray ionization mass spectrometry （HPLC-MS/ESI）. The positive ion SIM detection of levocarnitine （[M＋H] ＋, m/z= 162.1） used mildronate （[IM＋H] ＋, m/z= 147. l） as internal standard. The HPLC separation of the analytes was performed on a Ultimate XB-CN （4.6 mm×250 mm, 5 μm） column, with a flow rate of 1.0 mL-min-1. RESULTS The calibration curve was linear in the range of 0.4-12.8 mg.L-1 for levocamifine, with correlation coefficient above 0.99. The average extraction recovery was above 80%. The methodology recovery was above 92%, and below 114%. The intra-day and inter-day relative standard deviations were all less than 12%. The limit of detection （LOD） was 0.4 mg·L-1 for levocarnitine. CONCLUSION The method is accurate and simple for the determination of levocarnitine in human plasma.

关 键 词：左卡尼汀 高效液相色谱.质谱 血药浓度 

分 类 号：R696[医药卫生—泌尿科学]