魏绍峰;程寿峰;王兴宁;苟海潮;张爱华;
WEI Shaofeng;CHENG Shoufeng;WANG Xingning;GOU Haichao;ZHANG Aihua;School of Public Health,Guizhou Medical University;Key Laboratory of Environment Pollution Monitoring and Disease Control,Guizhou Medical University;Guizhou Entry-Exit Inspection and Quarantine Bureau;

• 1:贵州医科大学公共卫生学院
• 2:贵州医科大学环境污染与疾病监控教育部省部共建重点实验室
• 3:贵州出入境检验检疫局

摘要(Abstract)：

目的:建立测定大米中15种苯氧羧酸类除草剂农药残留量的气相色谱-四极杆飞行时间质谱(GCQ-TOF/MS)测定方法。方法:采用乙腈提取,Carbon固相萃取净化柱净化,三甲基硅烷化重氮甲烷衍生化,建立GC-Q-TOF/MS法测定大米中15种苯氧羧酸类除草剂[3,5-二氯苯甲酸、麦草畏、2-甲-4-氯苯氧丙酸(MCPP)、2-甲基-4-氯苯氧乙酸(MCPA)、2,4-滴丙酸(2,4-DP)、2,4-二氯苯氧乙酸(2,4-D)、5-氯苯酚、2,4,5-三氯苯氧丙酸(2,4,5-TP)、草灭平、2,4,5-三氯苯氧基乙酸(2,4,5-T)、2,4-滴丁酯(2,4-DB)、苯达松、地乐酚、毒秀定、三氟羧草醚)]含量的色谱条件、线性关系、检测限以及回收率,考察相对标准偏差,采用该法评价随机抽样的贵阳市售大米中15种苯氧羧酸类除草剂的含量。结果:本研究设定条件下15种苯氧羧酸类除草剂在20 min内完全分离,并测得相应的色谱峰;在0.05~1.0 mg/L范围内线性关系良好,相关系数为0.997 4~0.999 9;3个添加水平(0.05、0.1及0.15 mg/L)的平均回收率为80.1%~101.3%;精密度和重复性的相对标准偏差(RSD,n=5)为5.8%~9.6%;最低检出限(3S/N)在0.001~0.006 mg/kg;5种贵阳市售大米样品中未检出15种苯氧羧酸除草剂。结论:成功建立测定大米中15种苯氧羧酸类除草剂农药残留量的GC-Q-TOF/MS测定方法,贵阳市售大米中未检出15种苯氧羧酸类除草剂。
Objective: To test a GC-Q-TOF/MS method for determination of pesticide residue of 15 kinds of phenoxy-hydroxy-acid herbicides in rice. Methods: Study the chromatographic conditions,content of linearity,detection limit,recovery rate and relative standard deviationthe of detecting 15 kinds of phenoxy-hydroxy-acid herbicides in rice with acetonitrile extraction,Carbon SPE column purification,three methyl silane diazomethane derivatization and gas chromatography quadrupole time-offlight mass spectrometry(GC-QTOF MS). The 15 kinds of phenoxy-hydroxy-acid herbicides includes3,5-dichlorbenzoic acid,dicamba,MCPP,MCPA,2,4-DP,2,4-D,pentachlorophenol l,2,4,5-TP,chloramben,2,4,5-T,2,4-DB,bentazon,dinoseb,picloram,acifluorfen. The content of evaluation on sale in Guiyang,15 kinds of Phenoxyacid herbicides in rice. Then,the content of 15 kinds of phenoxy-hydroxy-acid herbicides in rice in Guiyang was evaluated by the above methods.Results: 15 kinds of phenoxy-hydroxy-acid herbicides were completly separated in 20 minutes. The linear relation was good between 0. 05 mg / L ~ 1. 0 mg / L under the mass spectroscopy condition andthe correlation was from 0. 997 4 to 0. 999 9. The mean recovery of three levels( 0. 05,0. 1,0. 15 mg / L)was from 80. 1% to 101. 3%,and the precision and repeatability of RSD values were from 5. 8% to 9.6%( n = 5). The detection line was between 0. 001 mg / kg and 0. 006 mg / kg. 15 kinds of phenoxy-hydroxy-acid herbicides were not detected in rice samples. Conclusion: The method is simple,rapid and with satisfactory recoveries that it can provide the scientific quarantine criterion for 15 kinds of phenoxyhydroxy-acid herbicides in rice. 15 kinds of herbicides were not detected in rice in Guiyang city.

关键词(KeyWords)： 气相色谱-四极杆飞行时间质谱;固相萃取;苯氧羧酸;除草剂;大米;贵阳
gas chromatography quadrupole time of flight mass spectrometry;solid phase extraction;phenoxy-hydroxy-acid;herbicide;rice;Guiyang

Abstract:

Keywords:

基金项目(Foundation):

作者(Author): 魏绍峰;程寿峰;王兴宁;苟海潮;张爱华;
WEI Shaofeng;CHENG Shoufeng;WANG Xingning;GOU Haichao;ZHANG Aihua;School of Public Health,Guizhou Medical University;Key Laboratory of Environment Pollution Monitoring and Disease Control,Guizhou Medical University;Guizhou Entry-Exit Inspection and Quarantine Bureau;

Email:

DOI: 10.19367/j.cnki.1000-2707.2016.11.012

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