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改进的QuEChERS气相色谱-串联质谱法测定草莓中21种杀菌剂残留
引用本文:侯雪,韩梅,邱世婷,胡莉,雷绍荣.改进的QuEChERS气相色谱-串联质谱法测定草莓中21种杀菌剂残留[J].农药学学报,2017,19(1):46-52.
作者姓名:侯雪  韩梅  邱世婷  胡莉  雷绍荣
作者单位:四川省农业科学院 分析测试中心/农业部农产品质量安全风险评估实验室(成都), 成都 610066
摘    要:采用改进的QuEChERS气相色谱-串联质谱法建立了检测草莓中21种杀菌剂(螺环菌胺、甲霜灵、四氟醚唑、酞菌酯、嘧菌环胺、戊菌唑、氟吡菌酰胺、氟菌唑、嘧菌胺、E-苯氧菌胺、抑霉唑、腈菌唑、醚菌酯、环氟菌胺、肟菌酯、丙环唑、环酰菌胺、氟环唑、咪唑菌酮、啶酰菌胺、嘧菌酯)残留的方法。样品经乙腈提取,采用N-丙基乙二胺(primary secondary amine,PSA)和石墨化碳黑(graphitized carbon blacks,GCB)作为分散固相萃取(dispersive solid phase extraction,DSPE)的吸附材料,净化液经氮气吹干、用V(正己烷):V(丙酮)=9:1混合溶液定容,采用气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)测定。结果表明:在质量浓度0.005~0.2 mg/kg范围内,21种杀菌剂与对应的峰面积间呈良好的线性关系;在0.01、0.05和0.1 mg/kg 3个添加水平下,21种杀菌剂的平均回收率均在70%~122%之间,RSD < 20%。该方法适用于草莓中21种杀菌剂残留的快速、高效和准确分析。

关 键 词:QuEChERS    气相色谱-串联质谱    草莓    杀菌剂    残留
收稿时间:2016/7/12 0:00:00
修稿时间:2016/11/18 0:00:00

Residues of 21 fungicides in Fragaria ananassa by modified QuEChERS and gas chromatography-tandem mass spectrometry
HOU Xue,HAN Mei,QIU Shiting,HU Li and LEI Shaorong.Residues of 21 fungicides in Fragaria ananassa by modified QuEChERS and gas chromatography-tandem mass spectrometry[J].Chinese Journal of Pesticide Science,2017,19(1):46-52.
Authors:HOU Xue  HAN Mei  QIU Shiting  HU Li and LEI Shaorong
Institution:Laboratory of Quality and Safety Risk Assessment for Agro-products (Chengdu), Ministry of Agriculture/Center of Analysis and Testing, Sichuan Academy of Agricultural Sciences, Chengdu 610066, China
Abstract:In order to determine 21 fungicides (spiroxamine, metalaxyl, tetraconazole, nitrothal-isopropyl, cyprodinil, penconazole, fluopyram, triflumizole, mepanipyrim, E-metominostrobin, imazalil, myclobutanil, kresoxim-methyl, cyflufenamid, trifloxystrobin, propiconazol, fenhexamid, epoxiconazole, fenamidone, boscalid, azoxystrobin) in Fragaria ananassa, the sample preparation method and GC-MS/MS analysis parameters were optimized. The sample was first extracted by acetonitrile. During the DSPE procedure, PSA and GCB were used as sorbents. After concentrated, the extract was dissolved by a mixed solvent V (hexane):V (acetone)=9:1. The extract was then determined with GC-MS/MS. Linear relationships between peak area and mass concentration of 21 fungicides were obtained in the range of 0.005-0.2 mg/kg. When the spiked levels were 0.01, 0.05 and 0.1mg/kg, the average recoveries all ranged from 70 to 122% with RSD < 20% (n=5). This method is suitable for the rapid and accurate detection of 21 fungicides in F. ananassa.
Keywords:QuEChERS  gas chromatography-tandem mass spectrometry  Fragaria ananassa Duch  fungicide  residue
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