基于TDESI-MS/MS法快速检测“焦糖色”非法染色中药  

Rapid Detection of Chinese Herbal Medicine Dyed by Caramel Color Based on TDESI-MS/MS

作　　者：李运 代伟[3] 高鹏 邵长春 王月玲 张虹艳 赵磊 LI Yun;DAI Wei;GAO Peng;SHAO Chang-chun;WANG Yue-ling;ZHANG Hong-yan;ZHAO Lei(Lanzhou Institutes for Food and Drug Control,Gansu Lanzhou 730000,China;Gansu Engineering Research Center for Monitoring Exogenous Harmful Residues in Traditional Chinese Medicines,Gansu Lanzhou 730000,China;Gansu Provincial Maternity and Childcare Hospital,Gansu Lanzhou 730050,China;Changchun University of traditional Chinese Medicine School of Medicine,Jilin Changchun 130117,China;Siping Institute for Food and Drug Control,Jilin Siping 136000,China)

机构地区：[1]兰州市食品药品检验检测研究院,甘肃兰州730000 [2]甘肃省种植中药材外源性污染物监测工程研究中心,甘肃兰州730000 [3]甘肃省妇幼保健院,甘肃兰州730050 [4]长春中医药大学药学院,吉林长春130117 [5]四平市食品药品检验所,吉林四平136000

出　　处：《中国药物评价》2022年第2期131-135,共5页Chinese Journal of Drug Evaluation

基　　金：甘肃省药品科研项目(2020GSMPA034)。

摘　　要：目的:采用热解吸电喷雾离子源质谱(thermal desorption electrospray ionization tandem mass spectrometry,TDESI-MS/MS)技术,建立中药中"焦糖色"非法染色的快速检测方法。方法:采用TDESI-MS/MS技术,以0.1%甲酸水溶液-甲醇(1∶1,v/v)为电喷雾溶液,设定电喷雾溶液流速140μL·h^(-1),热脱附温度230℃,正离子电喷雾离子化(ESI^(+));干燥气温度300℃;干燥气流速3 L·min^(-1);雾化器压力5psi;毛细管电压4000 V。采用多反应监测(multiple reaction monitoring,MRM)模式,以"焦糖色"生产中的副产物4-甲基咪唑为检测指标。样品经水提取,直接进样,与对照品的响应进行比较分析,确定是否存在"焦糖色"非法染色。结果:分别对19批次市售丁香、6批防风样品进行快速筛查,发现2批次丁香样品中检出4-甲基咪唑,存在"焦糖色"非法染色。结论:本方法操作简单、快速、灵敏,可用于中药中"焦糖色"非法染色的筛查。Objective:To develop a fast detecting method for caramel color illegally added into traditional Chinese medicinal materials by thermal desorption electrospray ionization tandem mass spectrometry(TDESI-MS/MS).Methods:The analysis was performed on TDESI-MS/MS,which was used to electrospray solution with 0.1%formic acid aqueous solution-methanol(1∶1,v/v).The electrospray solution flow rate of 140μL·h^(-1),and the thermal desorption temperature was 230℃.ESI^(+),set the dry gas temperature of 300℃and the flow rate of dry gas was 3 L·min^(-1).The atomizer pressure of 5psi and the capillary voltage of 4000 V.The detection was carried out by TDESI-MS/MS in the multiple-reaction monitoring(MRM)mode,it was used 4-methylimidazole as the detection index which was a by-product in caramel color production.The samples were extracted by water,directly injected.The judgement of whether dye was added or not was made by compared with the response of the standard substance.Results:To rapid screening of 19 batches of Caryophylli Flos and 6 batches of Saposhnikoviae Radix samples on the market,4-methylimidazole was discovered in 2 batches of Caryophylli Flos samples,and illegal caramel staining was identified.Conclusion:This method was simple,rapid and sensitive,which could be used to screen for illegal caramel staining in traditional Chinese medicine.

关 键 词：热解吸电喷雾离子源质谱技术 中药 焦糖色 4-甲基咪唑 

分 类 号：R284.1[医药卫生—中药学]