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中国精品科技期刊2020
戴尽波,沈洁,董文静,等. 微量QuEChERS-超高效液相色谱-串联质谱法检测凉茶中59种非法添加化学药物[J]. 食品工业科技,2024,45(6):242−253. doi: 10.13386/j.issn1002-0306.2023040213.
引用本文: 戴尽波,沈洁,董文静,等. 微量QuEChERS-超高效液相色谱-串联质谱法检测凉茶中59种非法添加化学药物[J]. 食品工业科技,2024,45(6):242−253. doi: 10.13386/j.issn1002-0306.2023040213.
DAI Jinbo, SHEN Jie, DONG Wenjing, et al. Determining the 59 Chemical Drugs Illegally Added in Herbal Tea by a Micro-QuEChERS-Based UPLC-MS/MS[J]. Science and Technology of Food Industry, 2024, 45(6): 242−253. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023040213.
Citation: DAI Jinbo, SHEN Jie, DONG Wenjing, et al. Determining the 59 Chemical Drugs Illegally Added in Herbal Tea by a Micro-QuEChERS-Based UPLC-MS/MS[J]. Science and Technology of Food Industry, 2024, 45(6): 242−253. (in Chinese with English abstract). doi: 10.13386/j.issn1002-0306.2023040213.

微量QuEChERS-超高效液相色谱-串联质谱法检测凉茶中59种非法添加化学药物

Determining the 59 Chemical Drugs Illegally Added in Herbal Tea by a Micro-QuEChERS-Based UPLC-MS/MS

  • 摘要: 目的:建立一种微量QuEChERS(micro-QuEChERS)结合超高效液相色谱-串联质谱(UPLC-MS /MS)同时检测凉茶中59种非法添加药物的分析方法。方法:样品用乙腈超声提取5 min,提取液用NaCl及无水Na2SO4进行盐析分层,上清液用C18吸附剂进行净化后,经ACQUITY HSS T3(100 mm×2.1 mm,1.8 μm)色谱柱分离,以0.01%甲酸水溶液(A)-乙腈:甲醇(8:2)(B)为流动相进行梯度洗脱,并采用电喷雾正负离子多反应监测模式检测,空白基质外标法定量。结果:59种化合物在其线性浓度范围内,线性关系良好,决定系数均大于0.999,检出限为5.0~10.0 μg/L,定量限为10.0~25.0 μg/L。在25.0、50.0、100.0 μg/L 3个添加水平下,平均回收率为60.3%~128.8%(n=6),相对标准偏差(RSD)1.0%~13.7%。结论:该方法操作简单,净化效果好,灵敏度高,可用于凉茶中59种非法添加化学药物的快速分析。

     

    Abstract: Objective: An analysis method for simultaneous determination of 59 kinds of chemical drugs illegally added in herbal tea by micro-QuEChERS method combined with ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) was established. Method: The samples were extracted by ultrasonic extraction from acetonitrile solution for 5 min and salted out with sodium chloride (NaCl) and anhydrous sodium sulfate (Na2SO4). Supernatant was purified with C18 sorbent and separated on a ACQUITY HSS T3 column (100 mm×2.1mm, 1.8 μm) by gradient elution using a mixture of 0.01% formic acid and acetonitrile:methanol (8:2) as the mobile phase. Then the analytes were quantified by UHPLC-MS/MS in multiple reaction monitoring mode (MRM) via positive and negative electrospray ionization quantified by external standard method. Result: The coefficient of determination of the standard calibration curves for the 59 analytes were all above 0.9990. The limit of detection (LOD, S/N≥3) and the limit of quantitation (LOQ, S/N≥10) were 5.0~10.0 and 10.0~25 μg/L. At three spiked of 25.0, 50.0 and 100.0 μg/L, the average recoveries of 59 analytes were 60.3%~128.8% (n=6) with the relative standard deviations in the range of 1.0%~13.7%. Conclusion: The method developed was simple, sensitive, and had good purification effect. It could be applied for the rapid determination of 59 chemical drugs illegally added in herbal tea.

     

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