基于QuEChERS法前处理的GC-MS检测梨中7种菊酯类农药残留
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摘要
[目的]建立一种同时测定梨中7种菊酯类农药的GC-MS方法。[方法]采用GC-MS法,QuEChERS法前处理梨样品,用乙腈溶液提取,PSA净化,对梨中7种菊酯类农药进行了多残留分析。[结果] 7种菊酯类农药在0.01～1.0 mg/L线性范围内,均呈现良好的线性关系,相关系数R2>0.9952;在0.01、0.1、0.5 mg/kg 3个加标质量分数下,各农药的平均回收率均在73.4%～106.0%之间,相对标准偏差在2.9%～7.8%之间。[结论]所建立的方法可以提供准确的定性和定量分析,操作简单、快速、灵敏度高,符合农药多残留检测要求,且所测梨的农药残留符合国家标准。
[Aims] To establish a GC-MS method for simultaneous determination of seven pyrethroid pesticides in pear.[Methods] Seven pyrethroid pesticide residues in pear were extracted with acetonitrile, purificated with PSA, and analyzed by GC-MS with QuEChERS. [Results] All the seven pyrethroid pesticides showed good linear relationship in the range of 0.01-1.0 mg/L with correlation coefficient R2> 0.9952. The recovery rates at 0.01, 0.1 and 0.5 mg/kg were between 73.4 and 106.0%, and the relative standard deviation was between 2.9 and 7.8%. [Conclusions] The established method can provide accurate qualitative and quantitative analysis. It is simple, rapid and sensitive. It meets the requirements of multi-residue detection of pesticides, and the pesticide residues in pear in the tested meet the national standards.
[Aims] To establish a GC-MS method for simultaneous determination of seven pyrethroid pesticides in pear.[Methods] Seven pyrethroid pesticide residues in pear were extracted with acetonitrile, purificated with PSA, and analyzed by GC-MS with QuEChERS. [Results] All the seven pyrethroid pesticides showed good linear relationship in the range of 0.01-1.0 mg/L with correlation coefficient R2> 0.9952. The recovery rates at 0.01, 0.1 and 0.5 mg/kg were between 73.4 and 106.0%, and the relative standard deviation was between 2.9 and 7.8%. [Conclusions] The established method can provide accurate qualitative and quantitative analysis. It is simple, rapid and sensitive. It meets the requirements of multi-residue detection of pesticides, and the pesticide residues in pear in the tested meet the national standards.
引文
[1]孙新菊,齐开杰,张绍铃,等.“鸭梨”“新高梨”果实发育中果肉及种子有机酸含量的变化[J].中国南方果树,2018,47(6):115-120.
[2]程暄生.拟除虫菊酯类杀虫剂及增效剂品种手册[M].南京:江苏省农药研究所,1993:1-415.
[3]胡艳,余术,陈聪,等.固相萃取-GC-ECD法测定草莓中的4种菊酯类农药[J].轻工科技,2018,34(5):113-114.
[4]KUANG Hua,MIAO Hong,HOU Xiao-lin,et al.Determination of Pyrethroid Residues in Pork Muscle by Immunoaffinity Clean-up and GC-ECD[J].Chromatographia,2009,70(5/6):995-999.
[5]王锦,刘世军,唐志书,等.气相色谱法检测大枣中联苯菊酯农药残留[J].陕西农业科学,2018,64(9):12-13.
[6]杨韶芸.气相色谱法测定蔬菜中5种拟除虫菊酯类农药的残留量[J].现代食品,2016,24(4):95-97.
[7]张兵,周向阳,胡祥娜,等.气相色谱-质谱联用仪测定蔬菜中十五种农药残留量[J].食品科学,2003,24(8):124-126.
[8]王姣.QuEChERS-气相色谱-串联质谱法测定茶叶中的多种拟除虫菊酯农药[J].现代食品,2018,15(3):121-125.
[9]荣维广,朱铭洪,何雨恬,等.新型QuEChERS技术气相色谱电子捕获检测器检测青菜中联苯菊酯和溴氰菊酯[J].农药,2018,57(8):589-592.
[10]高青珍.QuEChERS-色谱法快速测定蔬菜水果中的农药多残留(硕士论文)[D].北京:中国农业科学院,2014.
[11]姚德祥,黎小鹏,李拥军,等.QuEChERS前处理-气相色谱仪检测火龙果中的多种农药残留[J].仲恺农业工程学院学报,2017,30(1):36-41.
[12]何强,刘学芝,孔祥虹,等.超高效液相色谱-串联质谱法测定浓缩苹果汁中61种农药残留量[J].分析试验室,2015,34(3):300-306.
[13]国家卫生和计划生育委员会.GB 2763-2016.食品安全国家标准食品中农药最大残留限量[S].北京:中国标准出版社,2016.
[2]程暄生.拟除虫菊酯类杀虫剂及增效剂品种手册[M].南京:江苏省农药研究所,1993:1-415.
[3]胡艳,余术,陈聪,等.固相萃取-GC-ECD法测定草莓中的4种菊酯类农药[J].轻工科技,2018,34(5):113-114.
[4]KUANG Hua,MIAO Hong,HOU Xiao-lin,et al.Determination of Pyrethroid Residues in Pork Muscle by Immunoaffinity Clean-up and GC-ECD[J].Chromatographia,2009,70(5/6):995-999.
[5]王锦,刘世军,唐志书,等.气相色谱法检测大枣中联苯菊酯农药残留[J].陕西农业科学,2018,64(9):12-13.
[6]杨韶芸.气相色谱法测定蔬菜中5种拟除虫菊酯类农药的残留量[J].现代食品,2016,24(4):95-97.
[7]张兵,周向阳,胡祥娜,等.气相色谱-质谱联用仪测定蔬菜中十五种农药残留量[J].食品科学,2003,24(8):124-126.
[8]王姣.QuEChERS-气相色谱-串联质谱法测定茶叶中的多种拟除虫菊酯农药[J].现代食品,2018,15(3):121-125.
[9]荣维广,朱铭洪,何雨恬,等.新型QuEChERS技术气相色谱电子捕获检测器检测青菜中联苯菊酯和溴氰菊酯[J].农药,2018,57(8):589-592.
[10]高青珍.QuEChERS-色谱法快速测定蔬菜水果中的农药多残留(硕士论文)[D].北京:中国农业科学院,2014.
[11]姚德祥,黎小鹏,李拥军,等.QuEChERS前处理-气相色谱仪检测火龙果中的多种农药残留[J].仲恺农业工程学院学报,2017,30(1):36-41.
[12]何强,刘学芝,孔祥虹,等.超高效液相色谱-串联质谱法测定浓缩苹果汁中61种农药残留量[J].分析试验室,2015,34(3):300-306.
[13]国家卫生和计划生育委员会.GB 2763-2016.食品安全国家标准食品中农药最大残留限量[S].北京:中国标准出版社,2016.