液相色谱-串联质谱法测定保健食品中非法添加的18种镇静催眠类药物

Determination of 18 kinds of sedative and hypnotic drugs illegally added in health food by liquid chromatography-tandem mass spectrometry

中文关键词:  液相色谱-串联质谱法  保健食品  非法添加  镇静催眠类药物

英文关键词:liquid chromatography-tandem mass spectrometry  health foods  illegally added  sedative and hypnotic drugs

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)测定保健食品中非法添加的18种镇静催眠类药物的分析方法。方法 样品经甲醇超声提取, 采用C18(2.1 mm× 50 mm, 1.8 μm)色谱柱, 0.1%甲酸水溶液-甲醇为流动相, 梯度洗脱, 流速0.3 mL/min; 质谱检测器为ESI源(正离子)多反应监测模式进行定性、定量检测。结果 18种被测组分在5~100 ng/mL浓度范围内线性关系良好, 相关系数均大于0.999。5、20、50 ng/mL 3种添加浓度的平均回收率在77.6%~98.5%之间, 相对标准偏差为1.1%~5.5%。方法学检出限均低于0.2 μg/g。结论 该方法专属性强、灵敏度高、操作简便、测定快速, 可用于保健食品中非法添加的18种镇静催眠类药物的质量监控。

英文摘要:

      Objective To establish a method for the determination of 18 kinds of sedative and hypnotic drugs illegally added in health foods by ultra performance liquid chromatography-tandem triple quad mass spectrometry (UPLC-MS/MS). Methods Samples was extracted with methanol by ultrasound. C18 (2.1 mm×50 mm, 1.8 μm) chromatographic column was used for separation, with 0.1% formic acid aqueous solution-methanol as mobile phase, and gradient elution was performed at a flow rate of 0.3 mL/min. The mass spectrometry detector was ESI source, and the multiple reaction monitoring model was used for qualitative and quantitative detection. Results The linear relationship of 18 tested components was good in the range of 5?100 ng/mL concentration. The correlation coefficients were all greater than 0.999. The average recoveries were 77.6%?98.5%, and the relative standard deviation ranged from 1.1% to 5.5% at 3 spiked concentrations of 5, 20 and 50 ng/mL. The limits of detection of methodology were all lower than 0.2 μg/g. Conclusion This method has the advantages of high specificity, high sensitivity, simple operation and rapid determination, which can be used for quality control of 18 kinds of sedative and hypnotic drugs illegally added in health foods.