基于TDESI-MS/MS法快速检测“焦糖色”非法染色中药

中国药物评价 ›› 2022, Vol. 39 ›› Issue (2): 131-135.

基于TDESI-MS/MS法快速检测“焦糖色”非法染色中药

李运¹^，²，代伟³，高鹏¹^，²，邵长春¹^，²，王月玲¹^，²，张虹艳¹^，²，赵磊⁴^，⁵

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

收稿日期:2021-12-15 修回日期:2022-02-23 出版日期:2022-04-28 发布日期:2022-04-28
基金资助:
甘肃省药品科研项目(2020GSMPA034)

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

1.Lanzhou Institutes for Food and Drug Control, Gansu Lanzhou 730000, China；
2.Gansu Engineering Research Center for Monitoring Exogenous Harmful Residues in Traditional Chinese Medicines,
Gansu Lanzhou 730000, China; 3.Gansu Provincial Maternity and Childcare Hospital, Gansu Lanzhou 730050, China;
4.Changchun University of traditional Chinese Medicine School of Medicine，Jilin Changchun 130117, China； 5.Siping Institute for Food and Drug Control, Jilin Siping 136000, China

Received:2021-12-15 Revised:2022-02-23 Online:2022-04-28 Published:2022-04-28
Contact: zhao zhaolei E-mail:zhaolei0433@sina.com

摘要/Abstract

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140 μL·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4 000 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。

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

Abstract:

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 140 μL·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 4 000 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.

Key words: TDESI-MS/MS, Traditional Chinese medicine materials, Caramel color, 4-Methylimidazole

中图分类号:

R284.1

李运, 代伟, 高鹏, 邵长春, 王月玲, 张虹艳, 赵磊, .

基于TDESI-MS/MS法快速检测“焦糖色”非法染色中药 [J]. 中国药物评价, 2022, 39(2): 131-135.

LI Yun, DAI Wei, GAO Peng, SHAO Chang-chun, WANG Yue-ling, ZHANG Hong-yan, ZHAO Lei, .

Rapid Detection of Chinese Herbal Medicine Dyed by Caramel Color Based on TDESI-MS/MS [J]. CHINESE JOURNAL OF DRUG EVALUATION, 2022, 39(2): 131-135.

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