凝胶渗透色谱–气相色谱质谱法测定黑鱼品中敌敌畏
Determination of Dichlorvos in Snakehead by Gas Chromatography-Mass Spectrography Using Gel Penetrating Chromatogram

DOI: 10.12677/HJAS.2016.63007, PP. 43-48

Keywords: 敌敌畏，凝胶色谱净化，气相色谱–电子轰击离子源–质谱法
Dichlorvos, GPC, GC-EI-MS

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Abstract:

目的：对黑鱼中敌敌畏的检测方法进行优化。本文采用优化的样品前处理方法，通过凝胶色谱仪净化，利用气相色谱–电子轰击离子源–质谱法(GC-EI-MS)进行检测。敌敌畏在0.01~1 mg/L范围内具有良好的线性关系，相关系数为0.9999。敌敌畏农药残留的检出限为0.01 mg/kg。3个添加水平的回收率范围为73%~90%，相对标准偏差不大于10%。
Aim: To optimize the determination method of dichlorvos in snakehead. This paper was based on the optimization of sample pretreatment method, and then the supernatant was analyzed by gas chro- matography-mass spectrography using gel penetrating chromatogram. Calibration curves of dichlorvos were linear between 0.01 and 1 mg/L, with correlation coefficients of more than 0.9999. The limit of method detection is 0.01 mg/kg. Recoveries of the dichlorvos were in the range of 73%~90% with relative standard deviations of no more than 10% in a spiked concentration.

References

[1]	陈志涛, 陈春添, 赵建晖, 吴文凡, 郑香平, 张睿. 毛细管气相色谱同时测定水产品中多种农药残留量[J]. 福建分析测试, 2011, 20(6): 46-50.
[2]	贺小雨, 陈树兵, 俞雪钧, 樊苑牧, 诸静, 谢东华. 冷冻去脂–固相萃取/气相色谱–质谱法对水产品中禾草丹、溴氰菊酯及19种有机氯农药残留的测定[J]. 分析测试学报, 2009, 28(3): 306-309.
[3]	段建发, 林隆强, 林文华, 史佳虹, 林超. 凝胶色谱净化/气相色谱法测定鳗鱼中多种有机磷农药残留量[J]. 现代食品科技, 2012, 28(10): 1400-1402.
[4]	Kate, M. and Lehotay, S. (2003) Evaluation of Analyte Protectants to Improve Gas Chromatographic Analysis of Pesticides. Chromatography A, 1015, 163-184. http://dx.doi.org/10.1016/S0021-9673(03)01208-1
[5]	吴刚, 鲍晓霞, 王华雄, 俞春燕, 吴慧明, 叶庆富. 加速溶剂萃取–凝胶渗透色谱净化–气相色谱快速分析动物源性食品中残留的多种有机磷农药[J]. 色谱, 2008, 26(5): 577-582.

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