彭怡心，吴泽君，符春花^*，申 磊，楚 浩，刘小美

（株洲市食品药品检验所，湖南株洲 412000）

摘要：建立高效液相色谱-质谱联用法同时测定减肥类保健品中非法添加的12种化合物的方法。样品采用乙腈超声提取，经Welch Xtimate C18色谱柱（4.6 mm×150 mm，5 μm）分离，以0.1%甲酸-5 mmol/L乙酸铵水溶液（A）-乙腈（B）为流动相进行梯度洗脱，流速0.5 mL/min，柱温30 ℃。质谱采用电喷雾离子源正/负离子模式将样品离子化，并用多反应监测模式对12种化合物进行测定。12种化合物在各自考察范围内线性良好，相关系数均大于0.996 0；精密度和重复性的相对标准偏差分别为 2.1%～6.5%、2.1%～6.3%；高、中、低 3 种添加浓度的平均回收率范围为77.3%～120.9%；检出限为0.012～1.121 ng/mL，定量限为0.060～2.687 ng/mL。该方法灵敏度高、操作简便、结果准确，可用于减肥类保健品中12种非法添加物的同时测定。

关键词：高效液相色谱-质谱联用法；减肥类保健品；非法添加

中图分类号：TS207.3   文献标识码：A   文章编号：1674-506X（2021）06-0124-0008

Simultaneous Determination of 12 Kinds of Chemicals Illegally Added Into the Weight Controlling Health Food by High Performance Liquid Chromatography-mass Spectrometry

PENG Yi-xin, WU Ze-jun, FU Chun-hua^*, SHEN Lei, CHU Hao, LIU Xiao-mei

（Zhuzhou Institute for Food and Drug Control, Zhuzhou Hunan 412000, China）

Abstract：To establish a method to determinate 12 chemicals illegally added into the weight controlling health food simultaneously by high performance liquid chromatography-mass spectrometry(HPLC-MS). The samples were extracted with acetonitrile by ultrasonic processing and separated on a Welch Xtimate C18 (4.6 mm×150 mm, 5μm) column with 0.1% formic acid water solution (added 5 mmol/L ammonium acetate) (A) and acetonitrile (B) as the mobile phase by gradient elution at the flow rate of 0.5 mL/min, with the column temperature of 30 ℃. The samples were ionized by using positive/negative ion mode of electrospray ion source for mass spectrometry, and 12 compounds were determined by multi-reaction monitoring mode. The 12 compounds showed good linearity within their respective ranges,  and the correlation coefficients were all greater than 0.996 0. The relative standard deviations of precision and reproducibility were 2.1%～6.5% and 2.1%～6.3% , respectively. The average recoveries of the three additive concentrations of high, medium and low concentrations ranged from 77.3% to 120.9%. The limits of detection were 0.012～1.121 ng/mL and the limits of quantitation were 0.060～2.687 ng/mL. With the advantages of high sensitivity, simple operation and accurate results, the method can be used in simultaneous determination of 12 chemicals illegally added into the weight controlling health food.

Keywords：high performance liquid chromatography-mass spectrometry; weight controlling health food; illegally added

doi：10.3969/j.issn.1674-506X.2021.06-021

收稿日期：2021-06-16

作者简介：彭怡心（1992-），女，硕士。研究方向：食品质量安全检测与研究。

*通信作者

引文格式：彭怡心,吴泽君,符春花,等.高效液相色谱-质谱联用法同时测定减肥类保健品中12种非法添加物质[J].食品与发酵科技,2021,57(6):124-131.