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超高效液相色谱-串联质谱法测定茶叶、代用茶及调味茶制品中非法添加的63种化合物

[Determination of 63 compounds illegally added in tea, substitute tea and beverage foods by ultra-high performance liquid chromatography-tandem mass spectrometry].

作者信息

Tang Weiying, Huang Zewei, Qian Guangsheng, Wei Yutao, Huang Ying, Xu Xiaoping, Yu Xiaoqin

机构信息

Sichuan Provincial Institute for Food and Drug Control, Chengdu 610097, China.

West China School of Pharmacy, Sichuan University, Chengdu 610041, China.

出版信息

Se Pu. 2018 Dec 8;36(12):1245-1260. doi: 10.3724/SP.J.1123.2018.06025.

Abstract

A method based on ultra-high-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed for the simultaneous determination of 63 compounds illegally added in tea, substitute tea, and beverage products. The samples were extracted by ultrasonic extraction using methanol, and the analytes were separated on the Thermo Acclaim RSLC C18 chromatographic column (100 mm×2.1 mm, 2.2 μm) by gradient elution using 5 mmol/L ammonium formate solution containing 0.1% (v/v) formic acid and 0.1% (v/v) formic acid acetonitrile as the mobile phase. The electrospray ion source was operated in the positive ion mode using the dynamic multi-reaction monitoring (dMRM) method, and the results were quantified by the external standard method. The correlation coefficients () of the linear calibration curves were greater than 0.99 in the corresponding mass concentration ranges, and the limits of quantification (LOQs) for the analytes were 0.10-2.50 mg/kg. The average recoveries at three spiked levels ranged from 62.4% to 129.4%. The RSDs of the injection precision and the repeatability of samples were in the range 0.3%-9.6% (=6). Thus, the proposed method is simple, rapid, accurate, reliable, and applicable for the detection of the illegal addition of antipyretic and analgesic affect compounds in tea, substitute tea and beverage food.

摘要

建立了一种基于超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定茶叶、代用茶及饮料产品中63种非法添加化合物的方法。样品采用甲醇超声提取,以含0.1%(v/v)甲酸的5 mmol/L甲酸铵溶液和0.1%(v/v)甲酸乙腈为流动相,在Thermo Acclaim RSLC C18色谱柱(100 mm×2.1 mm,2.2 μm)上进行梯度洗脱分离分析物。采用电喷雾离子源正离子模式和动态多反应监测(dMRM)方法,结果用外标法进行定量。线性校准曲线在相应质量浓度范围内的相关系数()大于0.99,分析物的定量限(LOQ)为0.10 - 2.50 mg/kg。三个加标水平下的平均回收率为62.4%至129.4%。进样精密度和样品重复性的相对标准偏差(RSD)在0.3% - 9.6%范围内(n = 6)。因此,该方法简便、快速、准确、可靠,适用于茶叶、代用茶及饮料食品中非法添加解热镇痛类化合物的检测。

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