高效液相色谱-串联质谱法测定安神类保健品中的巴比妥

Rapid determination of barbital residues in sedative-hypnotic health products by high performance liquid chromatography- tandem mass spectrometry

中文关键词:  高效液相色谱-串联质谱法  保健品  安神药物  非法添加  巴比妥

英文关键词:high performance liquid chromatography-tandem mass spectrometry  health products  sedative-hypnotic medicines  illegal added  barbital

中文摘要:

      目的 建立高效液相色谱-串联质谱法测定安神类保健品中巴比妥残留的分析方法。方法 样品经甲醇-水溶液(50:50, V:V)超声提取、离心、过膜后, 经C18 色谱柱(50 mm×2.1 mm, 2.6 μm)分离, 以水和乙腈作为流动相, 梯度洗脱。在负电喷雾离子模式下, 采用多反应监测模式检测。结果 巴比妥在液体和固体基质中的绝对基质效应为4.97%~69.36%, 在1.0~50.0 ng/mL范围内线性均良好, 相关系数(r2)均在0.998以上。巴比妥在0.1、0.5和1.0 μg/g 3个水平的加标回收率为96.2%~112.0%, 相对标准标准偏差为0.10%~6.3% (n=6)。 结论 本方法操作简单、高效、可靠、灵敏度高, 能满足安神类保健品市场的监管和检验需求。

英文摘要:

      Objective To establish a method for the determination of barbital content in health products by high performance liquid chromatography-tandem mass spectrometry. Methods Samples were extracted with methanol-water (50:50, V:V) under ultrasonic condition, centrifuged by centrifugal machine and filtered by filtration, and separated on C18 chromatographic column (50 mm×2.1 mm, 2.6 μm). Gradient elution was carried out with water and acetonitrile as mobile phase. The determination was conducted in negative electrospray ionization mode under multiple reaction monitoring mode. Results The absolute matrixes effect of barbital for liquid and solid samples were 4.97%?69.36%. The linearity was good in the range of 1.0?50.0 ng/mL, with the correlation coefficients (r2) all above 0.998. The recoveries of all the illegal drugs in health products were 96.2%?112.0%, and the relative standard deviations were 0.10%?6.3% (n=6) at 0.1, 0.5, 1.0 μg/g, respectively. Conclusion This method is simple, efficient, reliable and sensitive, and can meet the supervision and inspection needs of the health care products market.