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| Simultaneous Determination of 90 Nafils in Distilled Liquor and Its Products by QuEChERS/High Performance Liquid Chromatography－Tandem Mass Spectrometry |
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| DOI： |
| KeyWord:high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） QuEChERS distilled liquor and its products nafils illegal addition |
| Author | Institution |
| CHEN Yan，YAN Li-juan，XU Dun-ming，LI Cui-yu，SUN Ting |
Xiamen Customs Technology Center，Xiamen ，China |
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| 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（r2） 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. |
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