UPLC-MS/MS法测定药用明胶硬空心胶囊中九种β-受体激动药残留量

Determination of Nine β-agonists in Medical Gelatin Hard Capsule Shells by UPLC-MS/MS

目的:建立同时测定药用明胶硬空心胶囊中9种β-受体激动药残留量的超高效液相-串联四级杆质谱方法(UPLCMS/MS)。方法:以多反应监测模式测定,以Waters ACQUITY UPLC~ BEH C_(18)柱进行分离,乙腈(含0.1%甲酸)-0.1%甲酸溶液梯度洗脱,流速:0.3 ml·min^(-1),离子化模式:ESI^+。结果:9种β-受体激动药线性范围0.25～5.00μg·kg^(-1),r为0.994 3～0.998 1;方法的最低检出浓度0.010～0.086μg·kg^(-1),回收率为70.01%～1 13.72%。结论:该方法快速、准确、灵敏,可作为同时测定药用明胶硬空心胶囊壳中9种β-受体激动药残留的方法。

Objective： To establish a method for the determination of nine β-agonists in medical gelatin hard capsule shells by a UPLC-MS/MS. Method： The multi-reactions monitoring （MRM） technology was used. The separation was performed on a,Waters AC- QUITY UPLC BEH C1s column with the mobile phase of acetonitrile（containing 0. 1% formic acid）-0. 1% formic acid with gadient elution and a flow rate of 0. 3 ml. min -1. Ion mode ： ESI ＋. Result. A linearity of nine 13-agonists was obtained from 0. 25 to 50. 00ug kg-1 （r = 0. 9943-0.9981 ）, respectively. The LODs of the method were between 0. 010 and 0.086 ug kg-1 and the average recoveries were 70.01%-113.72%. Conclusion： The method is rapid and sensitive, and＇ suitable for the determination of nine β-agonists in medi- cal gelatin hard capsule shells.