HPLC-ITMS法筛查医院制剂中非法添加糖皮质激素的研究  

Determination of Glucocorticoids Illegally Added in Preparations of Medical Institutions by HPLC-ITMS

作　　者：刘静 王震红 LIU Jing;WANG Zhen-hong(Liaoning Inspection,Examination&Certification Centre,Liaoning Institute for Drug Control,Liaoning Shenyang 110036,China)

机构地区：[1]辽宁省检验检测认证中心,辽宁省药品检验检测院,辽宁沈阳110036

出　　处：《中国药物评价》2024年第4期275-279,共5页Chinese Journal of Drug Evaluation

基　　金：辽宁省市场监督管理局科技计划项目(2022ZC006)。

摘　　要：目的:建立液相色谱-离子阱质谱联用(HPLC-ITMS)方法,检测糖皮质激素违法添加的15种化学成分。方法:采用乙腈作为提取溶剂,液相分离采用SHISEIDO CAPCELL-PAK C_(18)色谱柱,以0.2%冰醋酸水溶液-0.2%冰醋酸乙腈溶液为流动相进行梯度洗脱,流速为0.5 mL·min^(-1),柱温为25℃,质谱选择电喷雾离子源,在正离子扫描状态下以一级全扫描和二级全扫描方式进行检测。结果:15种化合物的色谱峰能够完全分离,方法的最低检出限为0.05~1.00 mg·kg^(-1)。20批抽检的医院制剂中,均未检出糖皮质激素成分。结论:本方法预处理简单且灵敏,具有良好专属性,可用于医院制剂中非法添加的15种糖皮质激素的定性筛查。Objective:A high performance liquid chromatography-ion trap mass spectrometry(HPLC-ITMS)method was developed for the rapid screening of 15 kinds of glucocorticoids illegally-added in the preparations of medical institutions.Methods:The samples were pre-processed with acetonitrile by vortex extraction,and separated on Shiseido CAPCELL-PAK C_(18)column by gradient elution with 0.2%acetic acid aqueous solution-0.2%acetic acid acetonitrile solution as mobile phases,and detected by MS and MS 2 after ionization with electrospray ionization source(ESI)in positive ion scanning mode.The column temperature was set to 25℃with flow rate of 0.5 mL·min^(-1).Results:The chromatographic peaks of 15 compounds can be completely separated with the developed HPLC-ITMS condition.The detection limits of this method are 0.05~1.00 mg·kg^(-1).No glucocorticoid ingredients were detected in the 20 batches of medical institution preparations.Conclusion:This method was specific,simple to operate,sensitive,and suitable for qualitative screening of 15 glucocorticoids illegally added to preparations of medical institutions.

关 键 词：医院制剂 糖皮质激素 违法添加 液相色谱-离子阱质谱联用法(HPLC-ITMS) 

分 类 号：R927.12[医药卫生—药学]