HPLC-Q-TOF/MS法快速筛查及定量分析辅助降血压类保健食品中的15种非法添加药物

目的： 建立高效液相色谱-四极杆飞行时间质谱（HPLC-Q-TOF/MS）快速筛查及定量分析辅助降血压类保健食品中常见的15种非法添加药物。方法： 样品以甲醇为提取溶剂进行超声提取，离心后取上清液，采用Waters HSS T3色谱柱（100 mm×2.1 mm，1.8 μm）进行分离，乙腈（含0.1%甲酸）和水（含10 mmol·L-1乙酸铵，0.1%甲酸）为流动相，梯度洗脱，流速为0.3 mL·min^-1，柱温30℃。质谱采用正负离子扫描，目标离子二级碎片扫描方式。根据对照品的色谱保留时间、一级质谱和二级质谱信息建立标准谱库。将样品信息入库比对，确定样品中是否添加了该化合物，并对阳性样品进行定量分析。结果： 15种化合物质量浓度在0.03~50 μg·mL^-1范围内线性相关系数均大于0.992，各类化合物的检测下限为0.01~2 μg·mL^-1，回收率为75.3%~110.5%，RSD为4.6%~9.9%。采用本方法对12种辅助降血压类保健食品进行了检测，3种无批号产品检出非法添加药物。结论： 该方法操作简单，分析时间短，灵敏度高，准确可靠，可用于保健食品中非法添加药物的筛查和定量。

Objective: To establish an HPLC-Q-TOF/MS method for the screening,confirmation and quantitation of 15 illegally added drugs in antihypertensive health foods. Methods: The target analytes in health food samples were extracted ultrasonically with methanol. After centrifugation,the supernatant was injected and the separation was performed on a Waters HSS T3 column(100 mm×2.1 mm,1.8 μm). Acetonitrile containing 0.1% formic acid and water containing 10 mmol·L^-1 ammonium acetate combined with 0.1% formic acid were used as mobile phase by gradient elution at a flow rate of 0.3 mL·min^-1,and the column temperature was set at 30℃. The analytes were detected by positive or negative ion ESI in Target MS/MS mode,while the potential positive samples were quantified. The chromatographic retention time,precursor ions and product ions were compared with the standards,and the samples that illegally adulterated were identified. Results: The linearities of all the 15 drugs ranged from 0.03 μg·mL^-1 to 50 μg·mL^-1 with the correlation coefficients of greater than 0.992. The limits of detection were between 0.01 and 2 μg·mL^-1 and the recoveries were in the range of 75.3% to 110.5%,with the relative standard deviations of 4.56% to 9.91%. Using this method, 12 kinds of antihypertensive health foods were tested, and 3 kinds of non-lotion products were detected to add illegal drugs. Conclusion: The HPLC-Q-TOF/MS method is rapid,accurate and selective,and it can be applied to the screening,confirmation and quantitation of 15 illegally added drugs in antihypertensive health foods.

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