Simultaneous Determination of 90 Nafils in Distilled Liquor and Its Products by QuEChERS/High Performance Liquid Chromatography－Tandem Mass Spectrometry

CHEN Yan; YAN Li-juan; XU Dun-ming; LI Cui-yu; SUN Ting

doi:10.19969/j.fxcsxb.23011301

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Simultaneous Determination of 90 Nafils in Distilled Liquor and Its Products by QuEChERS/High Performance Liquid Chromatography－Tandem Mass Spectrometry

Scientific Papers | 更新时间：2023-05-15

- Simultaneous Determination of 90 Nafils in Distilled Liquor and Its Products by QuEChERS/High Performance Liquid Chromatography－Tandem Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 5, Pages: 519-530(2023)
- 作者机构：
  
  厦门海关技术中心，福建厦门 361026
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23011301
  CLC：
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陈燕,严丽娟,徐敦明等.高效液相色谱－串联质谱法同时检测蒸馏酒及其配制酒中90种那非类物质[J].分析测试学报,2023,42(05):519-530.

CHEN Yan,YAN Li-juan,XU Dun-ming,et al.Simultaneous Determination of 90 Nafils in Distilled Liquor and Its Products by QuEChERS/High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(05):519-530.
陈燕,严丽娟,徐敦明等.高效液相色谱－串联质谱法同时检测蒸馏酒及其配制酒中90种那非类物质[J].分析测试学报,2023,42(05):519-530. DOI： 10.19969/j.fxcsxb.23011301.

CHEN Yan,YAN Li-juan,XU Dun-ming,et al.Simultaneous Determination of 90 Nafils in Distilled Liquor and Its Products by QuEChERS/High Performance Liquid Chromatography－Tandem Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(05):519-530. DOI： 10.19969/j.fxcsxb.23011301.

摘要

建立了QuEChERS/高效液相色谱－串联质谱法（QuEChERS/HPLC－MS/MS）同时测定蒸馏酒及其配制酒中90种那非类非法添加药物的分析方法。样品经甲醇提取后，采用基质分散固相萃取法（QuEChERS）进行净化；上清液过0.22 μm有机相微孔滤膜，以HPLC－MS/MS进行分析，采用电喷雾（ESI）离子源电离，正离子多反应监测模式（MRM）检测，保留时间和离子丰度比进行定性分析，外标法定量分析。以白酒、白兰地、人参酒作为基质，对方法的准确度和精密度进行验证。结果表明，在优化的色谱－质谱条件下，90种那非类物质20 min内可获得满意的分离和检测结果，在0.05 ~ 50 μg/L范围内线性关系良好，相关系数（,r,2,）均大于0.999，方法的检出限（LOD）为0.5 ~ 10.0 μg/kg，定量下限（LOQ）为1.25 ~ 25.0 μg/kg。各待测物在不同加标水平下的回收率为78.3% ~ 109%，相对标准偏差（RSD）为1.2% ~ 9.9%。采用该方法测定47批蒸馏酒及其配制酒中90种那非类物质，结果显示，2批次样品中检出西地那非。该方法前处理简便，净化效果好，回收率稳定，可用于蒸馏酒及其配制酒中90种那非类非法添加药物的同时快速检测。

Abstract

A QuEChERS/high performance liquid chromatography－tandem mass spectrometry （HPLC－MS/MS） was established for the determination of 90 nafils illegally added into distilled liquor and its products．The distilled liquor and its products samples were extracted with methanol solution，followed by purification of matrix dispersion solid phase extraction．The supernatant was firstly passed through a 0.22 μm organic phase microporous filter membrane，then analyzed by liquid chromatography－tandem mass spectrometry with electrospray ionization（ESI） ion source in positive ion mode under multi-reaction monitoring（MRM） mode．The retention time and ion ratio were used for qualitative analysis and the external standard method was adopted for quantification．The accuracy and precision of the method were verified by taking white spirit，Brandy and ginseng wine as sample matrices．The results showed that 90 kinds of illicit drugs could be satisfactorily separated within 20 min under the above chromatographic and mass spectrometric conditions，and the linearities were good in the range of 0.05－50 μg/L，with correlation coefficients（,r,2,） greater than 0.999．The limits of detection（LODs） of the method were in the range of 0.5－10.0 μg/kg，and the limits of quantitation（LOQs） were 1.25－25.0 μg/kg．The recoveries for the analytes at different spiked levels ranged from 78.3% to 109%，with relative standards deviations（RSDs） of 1.2%－9.9%．The method was applied to the determination of 90 nafils in 47 batches of distilled liquor and its products．The results showed that sildenafil is contained in 2 batches of samples．With the advantages of simplicity in pretreatment，good purification effect on complex liquor matrix，and stable recovery，this method could be used for the rapid and simultaneous detection of 90 nafils illegally added substances in distilled liquor and its products.

关键词

高效液相色谱－串联质谱法QuEChERS蒸馏酒及其配制酒那非类物质非法添加

Keywords

high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）QuEChERSdistilled liquor and its productsnafilsillegal addition

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