辽宁省分析科学研究院
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王璐, 刘成雁, 王志嘉, 等. 保健食品中9种镇静催眠类药品的UPLC-MS/MS法检测及质谱裂解特征的研究[J]. 分析测试学报, 2016,35(2):219-224.
Simultaneous Determination of 9 Kinds of Sedative Hypnotic Drugs in Health Foods Using UPLC-MS/MS and ESI Fragmentation Studies[J]. 2016,35(2):219-224.
建立了同时测定保健食品中9种镇静催眠类化合物(氯美扎酮、三唑仑、阿普唑仑、艾司唑仑、地西泮、硝西泮、奥沙西泮、劳拉西泮、氯氮卓)的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法,并研究了其质谱裂解规律。样品以甲醇为提取溶剂,经Zorbax SB-C18(3.5 μm,2.1 mm×150 mm)色谱柱分离,乙腈-水(含0.1%甲酸)为流动相梯度洗脱,流速为0.3 mL/min。采用电喷雾离子源(ESI),正离子多反应监测(MRM)扫描方式检测,基质匹配标准曲线法定量。9种药物在0.5~50 μg/L范围内线性关系良好,相关系数(r2)均大于0.99,定量下限为1.6~9.2 μg?kg-1。低、中、高3个加标水平下的平均回收率为78.1%~101.2%,日内相对标准偏差(RSD)为1.4%~9.7%,日间RSD为2.0%~11.2%。该法简便、快速、准确可靠,适合于保健食品中非法添加镇静催眠类药品的高通量筛查。而对目标化合物碎片离子及质谱裂解规律的研究,也为其定性鉴别和定量分析提供了参考。
An ultra high performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the determination of 9 sedative hypnotic drugs(chormezanone,triazolam,alprazolam,estazolam,diazepam,nitrazepam,oxazepam,lorazepam,chlordiazepoxide) in health foods, and the dissociation pathways of nine drugs were studied by electrospray ion mass spectrometry.After extracted with methanol,the analyses were separated on a Zorbax SB-C18(3.5 μm,2.1 mm×150 mm) chromatographic column by gradient elution using a mixture of acetonitrile and 0.1% formic solution as mobile phase at a flow rate of 0.3 mL/min.Detection was performed by electrospray ionization in the positive ion mode under multiple reaction monitoring(MRM) mode,and quantified with matrix standard curve.As a result,the calibration curves for all target compounds were linear in the range of 0.5-50 μg/L with correlation coefficients(r2) larger than 0.99.The limits of quantitation(LOQ,S/N≥10) were in the range of 1.6-9.2 μg?kg-1.The recoveries for all the drugs were 78.1%-101.2%.The intra and inter day precisions values at three spiked levels were between 1.4%-9.7%and 2.0%-11.2%,respectively.With strong selectivity,high sensitivity,easy operation and rapid detection,this method could be used to detect 9 kinds of illegally added sedative drugs in health foods.Moreover,the study of mass spectrometric behaviours and ion fragmentation patterns of nine drugs could provide a reference for the qualitative identification and quantitative analysis.
超高效液相色谱-串联质谱保健食品镇静催眠类质谱裂解
ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)functional foodssedative hypnotic drugsfragmentation
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