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固相萃取-气相色谱-串联质谱法测定葡萄酒中六种吡唑类杀菌剂

Determination of Six Pyrazole Fungicides in Grape Wine by Solid-Phase Extraction and Gas Chromatography-Tandem Mass Spectrometry.

作者信息

Shen Yan, Li Zhou, Ma Qiang, Wang Chuanxian, Chen Xiangzhun, Miao Qian, Han Chao

机构信息

College of Chemistry and Materials Engineering, Wenzhou University , Wenzhou, Zhejiang 325035, People's Republic of China.

Wenzhou Entry-Exit Inspection and Quarantine Bureau of People's Republic of China , Wenzhou, Zhejiang 325027, People's Republic of China.

出版信息

J Agric Food Chem. 2016 May 18;64(19):3901-7. doi: 10.1021/acs.jafc.6b00530. Epub 2016 May 3.

Abstract

A gas chromatography-tandem mass spectrometry (GC-MS/MS) method was developed for the first simultaneous identification and quantification of six pyrazole fungicides (furametpyr, rabenzazole, fluxapyroxad, penflufen, bixafen, and isopyrazam) in grape wine samples. The grape wine samples were first diluted with water, then purified by solid-phase extraction, and finally examined by GC-MS/MS in multiple reaction monitoring (MRM) mode. Matrix-matched calibration curves were used to correct the matrix effects. The limits of quantification (LOQs), calculated as 10 times the standard deviation, were 0.2-0.8 μg kg(-1) for the six pyrazole fungicides. The average recoveries were in the range of 74.3-94.5%, with relative standard deviations (RSDs) below 5.8%, measured at three concentration levels. The proposed method is suitable for the simultaneous determination of six pyrazole fungicides in grape wine samples.

摘要

建立了一种气相色谱-串联质谱(GC-MS/MS)方法,用于首次同时鉴定和定量葡萄酒样品中的六种吡唑类杀菌剂(呋嘧磺隆、苯并异唑腈、氟唑菌酰胺、戊苯吡菌胺、联苯吡菌胺和异吡唑酰胺)。葡萄酒样品先用水稀释,然后通过固相萃取进行净化,最后采用多反应监测(MRM)模式的GC-MS/MS进行检测。采用基质匹配校准曲线校正基质效应。六种吡唑类杀菌剂的定量限(LOQ)以标准偏差的10倍计算,为0.2-0.8μg kg(-1)。在三个浓度水平下测得的平均回收率在74.3-94.5%范围内,相对标准偏差(RSD)低于5.8%。所提出的方法适用于同时测定葡萄酒样品中的六种吡唑类杀菌剂。

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