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

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作  者:朱韵洁[1,2] 杨钊[2] 李新荣[2] 曹志胜[2] 孙勇[1] 

机构地区:[1]青岛大学医学院药学系,山东青岛266021 [2]青岛市药品检验所

出  处:《中国药师》2012年第1期17-20,共4页China Pharmacist

摘  要: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.

关 键 词:β-受体激动药 药用明胶硬空心胶囊 超高效液相色谱-串联四极杆质谱 

分 类 号:R917[医药卫生—药物分析学]

 

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