LC-MS/MS法分析保健品及中成药中添加的15种镇静催眠剂___

 

 

 

 

目的：建立保健品及中成药中非法添加15种镇静催眠剂的LC-MS/MS分析方法。方法：采用Waters 2695/Quattro Micro液质联用仪，以Kromasil 100-3.5 C₁₈（150 mm×2.1 mm，3.5 μm）色谱柱为固定相，0.1%甲酸–甲醇为流动相，梯度洗脱，流速为0.2 mL·min^-1；质谱检测器采用ESI电离源，以正离子和MRM方式进行检测；供试样品的处理，采用以甲醇为溶剂的超声提取方法。结果：15种被测组分线性关系良好（r=0.9978~0.9998，n=8）；3种浓度的平均添加回收率为76.2%~108.1%（RSD 1.6%~11.6%,n=6）；混合标准溶液3 d重复进样峰面积的RSD为1.4%~7.1%（n=9）；最低检测限为0.2~5.9 pg。结论：本方法结果准确、灵敏度高、重复性好，适用于保健品及中成药非法添加镇静催眠剂的质量监控。

 

 

 

Objective:To establish a LC-MS/MS method for analysis of 15 sedatives and soporifics illegally added into functional foods and traditional Chinese medicine preparations.Methods:The analysis was performed by a LC-MS/MS system of Waters 2695/Quattro Micro,using Kromasil 100-3.5 C₁₈ (150 mm×2.1 mm,3.5 μm) column as stationary phase and 0.1% formic acid – methanol system as mobile phase.The gradient elution was done with a flow rate of 0.2 mL·min^-1.Positive ionization was adopted during the MRM procedure using ESI source.A sonic-bath was used to process samples with methanol as the solvent.Results:Good linear relationship was obtained in the analysis of the 15 components of interest (r=0.9978-0.9998,n=8).The average spiked recoveries of three levels of concentration were 76.2%-108.1% (RSD was 1.6%-11.6%,n=6).RSD of peak area of mixed standard solution were 1.4%-7.1% (n=9),which was repeatedly injected in 3 days.The limits of detection of 15 components were within 0.2-5.9 pg.Conclusions:The method is accurate,sensitive,repetitive,and appropriate to control the quality of functional foods and traditional Chinese medicine preparations,into which sedative-hypnotic drugs were illegally added.