液相色谱-串级质谱法同时检测中成药及保健食品中非法添加的22种苯二氮卓类药物

Simultaneous Determination of 22 Benzodiazepines in Chinese Patent Drugs and Health-Care Foods by Liquid Chromatography-Tandem Mass Spectrometry

建立了同时检测中成药及保健食品中22种苯二氮卓类药物的液相色谱-串级质谱(LC-MS/MS)方法。在硼砂缓冲液(pH 11)中,样品中的苯二氮卓类药物经乙醚-二氯甲烷(8∶2,V/V)提取,浓缩至干后,用乙腈-水(2∶8,V/V)溶解残渣,采用电喷雾正离子模式电离(ESI+),多反应监测定性和同位素标记的内标物进行内标法定量。结果表明:在0.5～50.0%g/L范围内,22种苯二氮卓类药物的线性相关系数均大于0.9990;检出限为0.0085～0.062%g/L;定量限为0.028～0.21%g/L。添加浓度水平为1.0,2.0和5.0%g/kg时,平均回收率为58.0%～116.5%;相对标准偏差为2.4%～12.2%。

A sensitive liquid chromatography-tandem mass spectrometric（LC-MS/MS） method has been developed for simultaneous determination of 22 benzodiazepines in Chinese patent drugs and health-care foods samples.Compounds were extracted with ether-dichloromethane（8 ∶ 2,V/V） in pH 11 borax buffer solution,the extract was concentrated to dry,dissolved in acetonitrile：water（2 ∶ 8,V/V）,detected by positive electrospray ionization tandem mass spectrometry in the multiple reaction monitoring（MRM） mode,and quantified by isotope internal standard method.There were good linear correlations between the peak areas and concentration of the 22 benzodiazepines,the linear range was 0.5-50.0 L and correlation coefficients were above 0.9990.The limits of detection（LOD） of these 22 benzodiazepines were in the range of 0.0085-0.062 L,limits of quantification（LOQ） were in the range of 0.028-0.21 L.The average recoveries of benzodiazepines were 58.0%-116.5%,at spiked levels of 1.0,2.0 and 5.0 kg,the relative standard deviations（RSDs） of the method were between 2.4% and 12.2%.