食品科学 ›› 2022, Vol. 43 ›› Issue (10): 336-341.doi: 10.7506/spkx1002-6630-20210204-080

• 安全检测 • 上一篇    

超高效液相色谱-高分辨质谱快速筛查和确证凉茶中56 种非法添加药物

刘桂联,陈茹,罗小宝,陈均正,朱嘉仪   

  1. (1.广东省食品工业研究所有限公司,广东 广州 511442;2.广东省食品工业公共实验室,广东 广州 511442;3.广东省质量监督食品检验站,广东 广州 511442)
  • 出版日期:2022-05-25 发布日期:2022-05-27
  • 基金资助:
    江门市科技计划项目(2020030101110005138)

Rapid Screening and Confirmation of 56 Illegally Added Drugs in Herbal Tea by Ultra-high Performance Liquid Chromatography-High Resolution Mass Spectrometry

LIU Guilian, CHEN Ru, LUO Xiaobao, CHEN Junzheng, ZHU Jiayi   

  1. (1. Guangdong Food Industry Institute Co. Ltd., Guangzhou 511442, China; 2. Guangdong Provincial Public Laboratory of Food Industry, Guangzhou 511442, China; 3. Guangdong Food Quality Supervision and Inspection Station, Guangzhou 511442, China)
  • Online:2022-05-25 Published:2022-05-27

摘要: 采用超高效液相色谱-高分辨质谱联用技术,建立快速筛查和确证凉茶中56 种非法添加药物的分析方法。样品用甲醇提取后,经Accucore RP-MS色谱柱(100 mm×2.1 mm,2.6 μm)进行梯度分离,采用全扫描-数据依赖二级扫描模式采集数据进行快速筛查确证并测定含量。56 种非法添加药物在2~100 μg/L质量浓度范围内呈良好线性关系,相关系数(R2)均大于0.99,3 种加标水平的平均回收率为90.4%~105.0%,相对标准偏差均不大于6.0%,检出限为0.5~2.5 μg/L,定量限为1.5~8.0 μg/L。该方法具有快速、准确度高、灵敏度高、可同时进行筛查和含量测定等优点,可用于凉茶非法添加药物的快速筛查和确证。

关键词: 超高效液相色谱;高分辨质谱;非法添加;快速筛查;凉茶

Abstract: A rapid screening method for 56 illegally added drugs in herbal tea was developed by ultra-high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS). The samples were extracted with methanol and separated on an Accucore RP-MS column (100 mm × 2.1 mm, 2.6 μm) by gradient elution. A full mass scan/data dependent MS2 (Full MS/dd MS2) mode was used to collect data for rapid screening and confirmation. The correlation coefficients (R2) of the calibration curves of the analytes were all greater than 0.99 in the concentration range of 2–100 μg/L. The average recoveries ranged from 90.4% to 105.0% at three different spiked levels with relative standard deviations (RSDs) not more than 6.0%, the limits of detection were between 0.5 and 2.5 μg/L, and the limits of quantification were between 1.5 μg/L to 8.0 μg/L. This method was rapid, accurate and sensitive, and it was suitable for simultaneous screening and quantitation. It can be used for rapid screening and confirmation of illegal additives in herbal tea.

Key words: ultra-high performance liquid chromatography; high resolution mass spectrometry; illegal additives; rapid screening; herbal tea

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