LC-MS/MS测定人血浆中的罗红霉素

Determination of Roxithromycin in human plasma by LC-MS/MS

目的采用液相色谱一质谱法测定人血浆中的罗红霉素。方法采用API3000型LC—MS／MS液质联用系统。Uhimate C18分析柱（50mm×4．6mm，5μm），流动相为甲醇-水（80：20，含0．1％甲酸），流速0．3ml·min-1。MRM模式检测（离子对837．5／679．5），内标法定量。结果罗红霉素和内标的保留时间分别为2．39、2．36min，标准曲线0．01～10．00μg·ml-1的线性良好，最低定量限为10ng·L-1，日内、日间RSD分别小于3．4％、2．6％，方法回收率98．8％-106．6％，萃取回收率70．7％～73．7％。结论所建方法快速简便、灵敏准确，适用于血浆中罗红霉素浓度的测定及药物动力学研究。

OBJECTIVE To establish an RP - HPLC - MS/MS method for determination of Roxithromycin （RM） in human plas- ma. METHODS The assay was conducted with an API 3000 LC - MS/MS system consisted of a Ultimate C18 column （50 mm× 4.6 mm ,5 μm）. The mobile phase of methanol- water （80 ： 20, with 0.1% formic acid） was pumped at 0.3 ml. min- 1 through the col- umn. MRM mode （ ion pair was 837.5/679.5 ） was used for the detection. RESULTS The retention time for RM and internal standard （Clarithromycin） were 2.39 rain and 2.36 min, respectively. A linearity of romithromycin curve was within 0.01 - 10.00 μg.L-1. The lowest concentration of detection in plasma was 10 ng. L- 1. The intra - day RSD and inter - day RSD were less than 3.4% and 2. 6% ,respectively. The method recovery was 98.8% - 106.6%. The extract efficiency was 70.7% - 73.7%. CONCLUSION The method with mass detection was found to be simple, rapid and sensitive, and was accurate for determination of RM in human plasma.