超高效液相色谱-串联质谱法检测扶正解毒散剂中非法添加物喹乙醇、乙酰甲喹

Determination of Olaquindox and Mequindox Illegally Added in Fuzhengjiedusan by UPLC-MS/MS

Key words:  olaquindox  mequindox  Fuzhengjiedu san  UPLC-MS/MS

摘要:

建立了扶正解毒散中非法添加喹乙醇、乙酰甲喹检测的UPLC-MS/MS方法。样品经60%乙腈提取稀释后,采用ACQUITY UPLC^R BEH C18色谱柱为分离柱,质谱正离子扫描分析测定。结果显示,喹乙醇、乙酰甲喹在5～200 ng/mL的范围内线性关系良好(R²=0.9984,R²=0.9995)；样品检出限为25μg/mL,定量限为50μg/mL。在80、100、120μg/mL添加水平的回收率为90%～103%,批内批间变异系数均小于10%。本方法灵敏、快速、重现性好,适用于扶正解毒散中非法添加喹乙醇、乙酰甲喹的检测。

Abstract:

A method was established for determination of Olaquindox and Mequindox illegally added in Fuzhengjiedusan by UPLC-MS/MS. The sample was extracted and diluted with 60% acetonitrile,the ACQUITY UPLCR BEH C18 was used as the separation column, and the determination was conducted by scanning positive ion by mass spectrometry. The results showed that the good linear range was 5 to 50 ng/mL(R_²=0.9984,R_²=0.9995).The detection limit was 2μg/mL, and the quantitation limit was 5μg/m L.The analysis of spiked 80、100、120μg /mL olaquindox and mequindox showed that the recoveries ranged from 90% to 103% and the relative standard deviations were below 10%. The experiment showed that the method was reliable, sensitive and reproducibility and suitable for the determination of olaquindox and mequindox illegally added in Fuzhengjiedusan.