摘要
目的:建立同时测定蛇酒中醋酸泼尼松、醋酸氢化可的松、醋酸地塞米松、布地奈德和甲泼尼龙的快速高分离液相色谱-电喷雾质谱联用方法。方法:采用Agilent Poroshell 120 EC-C18色谱柱(100mm×3mm,2.7μm),乙腈(含0.1%甲酸)-0.1%甲酸水溶液为流动相进行梯度洗脱,流速0.3m L/min;采用电喷雾离子源,以正离子、多反应监测扫描模式对蛇酒中的5种糖皮质激素进行定性定量检测,并对其裂解方式进行解析。结果:醋酸泼尼松、醋酸氢化可的松、醋酸地塞米松、布地奈德和甲泼尼龙线性关系良好,R2均>0.99,8种蛇酒中检测到糖皮质激素。结论:本研究建立的快速高分离液相色谱-电喷雾质谱联用法方便快捷、灵敏度好、准确度高,适用于蛇酒中非法添加成分的定性定量检测。
Objective: To establish a rapid resolution liquid chromatography-electrospray ionization-mass spectrometry(RRLC-ESI-MS) method for prednisone acetate,hydrocortisone acetate,dexamethasone acetate,budesonide and methylprednisolone,which were illegally added in snake wine.Methods: The content determination of the five compounds was performed on Agilent Poroshell 120 EC-C18 column(100 mm×3 mm,2.7μm).The mobile phase consists of acetonitrile(containing 0.1% formic acid) and 0.1% formic acid solution,gradient elution with flow rate of 0.3 m L/min.The MS conditions: electrospray ionization(ESI) source,with positive ion,multiple reaction monitoring(MRM) mode to detect prohibited substances in snake wine.In addition,we also analyzed the cracking mode of five glucocorticoids.Results: The linear range of prednisone acetate,hydrocortisone acetate,dexamethasone acetate,budesonide and methylprednisolone were good in the range respectively,with the R2>0.99,and glucocorticoids were found in eight samples.Conclusion: The method established by the study is fast,convenient,high sensitivity and high accuracy,which could detect prohibited substances quantitatively and qualitatively in snake wine.
出处
《中华中医药杂志》
CAS
CSCD
北大核心
2017年第12期5628-5632,共5页
China Journal of Traditional Chinese Medicine and Pharmacy
基金
浙江省自然科学基金项目(N o.L Y14H270014)
浙江省公益性技术应用研究计划项目(No.2016C33086)
浙江中医药大学校级科研基金项目(No.711200F017)
浙江中医药大学基础医学院"中医证的本质研究"创新团队(No.JCIT2016-3)~~
