LC-MS/MS法测定匹多莫德的血浆浓度及其应用

Determination of pidotimod in human plasma by LC-MS/MS and its application

目的建立LC-MS/MS法测定匹多莫德的血浆浓度。方法用舒巴坦作为内标,采用乙腈沉淀蛋白进行样本处理,通过CAPCELL PAK C_(18)(50 mm×2.0 mm,5μm)色谱柱进行分离,以5 mmol·L^(-1)乙酸铵溶液-乙腈-乙酸(94.6:5:0.4)作为流动相进行等度洗脱,流速为0.2 mL·min^(-1),采用电喷雾进行离子化,用负离子扫描进行MRM分析,全部分析时间为4 min。结果匹多莫德在44.7~44 700μg·L^(-1)内线性良好(r=0.999 4,n=10)。批内、批间精密度好(RSD均<15%),提取回收率为88.93%~94.49%。结论本法重复性以及专一性均较好,可用于匹多莫德的药动学研究以及测定需求。

AIM To establish an LC-MS/MS method for determination of pidotimod in human plasma.METHODS Sulbuctam was used as the internal standard.Acetonitrile was used to pretreat plasma samples,analysis was carried out on a CAPCELL PAK C_(18)(50 mm×2.0 mm,5 μm) column with a mobile phase composed of 5 mmol·L^(-1) ammonium acetate solution-acetonitrile-acetic acid(94.6:5:0.4) with the speed of 0.2 mL·min^(-1).The detection was performed on a triple quadrupole tandem mass spectrometer by MRM via electrospray ionization(ESI) source in negative mode.The whole analytical time was 4 min.RESULTS The method had a good linear range between 44.7-44 700μg·L^(-1)(r=0.999 4,n=10).RSD values of inter- and intra- batch precision were all below 15%.Values of extraction recovery were from 88.93% to 94.49%.CONCLUSION The LC-MS/MS method has been proved to have good reproducibility,specificity and to be suitable for pharmacokinetic research and determination of pidotimod.