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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。
Objective To establish a HPLC-MS / MS method for the determination of plasma concentration of pidotimod. Methods Sulbactam was used as an internal standard and the proteins were precipitated by acetonitrile. The samples were separated by CAPCELL PAK C_ (18) (50 mm × 2.0 mm, 5 μm) column and eluted with 5 mmol·L -1 ammonium acetate Acetonitrile-acetic acid (94.6: 5: 0.4) was used as mobile phase. The flow rate was 0.2 mL · min ~ (-1), ionization was performed by electrospray and MRM analysis was performed by negative ion scan. For 4 min. Results Pidotimod was linear in 44.7-44 700 μg · L -1 (r = 0.999 4, n = 10). The intra-and inter-batch precision was good (RSD <15%), and the extraction recovery was 88.93% ~ 94.49%. Conclusion This method is good reproducibility and specificity, can be used for pharmacokinetics of pidotimod and determination of demand.