摘要
目的:建立UPLC-MS/MS法检测中药制剂中非法添加的13种抗组胺类药物。方法:样品经甲醇超声提取后,经Waters ACQUITY UPLC BEH C18(2.1 mm×150 mm,1.7μm)色谱柱分离,以10 mmol/L甲酸铵-0.1%甲酸水和甲醇为流动相,梯度洗脱,采用电喷雾离子(ESI)源,正离子扫描,多反应监测(MRM)模式检测。结果:13种抗组胺类成分呈良好线性关系,r均大于0.999,检出限为0.55~0.66 ng/mL,平均加标回收率为91.1%~101.3%,RSD均小于5%。结论:该方法准确、可靠,可用于中药制剂中非法添加抗组胺类成分的定性定量分析。
Objective:To determine 13 kinds of antihistam illegally added in raditional Chinese medicine preparations by UPLC-MS/MS. Methods:After ultrasonic extraction with methanol,the samples were separated on a Waters ACQUITY UPLC BEH C18 column(2.1 mm×150 mm,1.7 μm)with 10 mmol/L ammonium formate-0.1% formic acid solution and methanol as the mobile phase and gradient elution. Electrospray ionization(ESI)source in positive ion mode was used to analyze 13 kinds of antihistam in the multiple reaction monitoring(MRM)mode. Results:All 13 kinds of antihistam showed a good linear relationship,r were greater than 0.999,the detection limits were 0.55~0.66 ng/mL,the average sample recovery was 91.1%~101.3%,and the RSDs were less than 5%. Conclusion:The establish method is accurate and reliable,which can be used for the qualitative and quantitative analysis of antihistam illegally added in traditional Chinese medicine preparations.
作者
王超
姜鑫
矫筱蔓
陈权
WANG Chao JIANG Xin;JIAO Xiao-man;CHEN Quan(Liaoning Institute for Drug Control,Shenyang 110036,China)
