摘要
建立了气相色谱测定鸡蛋中氟虫腈的检测方法。样品经过乙腈/水提取、HLB固相萃取柱净化、气相色谱外标法测定表明,氟虫腈在0.000 5~0.064 0μg/m L内具有较好线性关系,线性相关系数0.999 85,方法检出限0.6μg/kg,加标回收率73.4%~84.2%,RSD值6.1%~8.6%。该方法前处理简单快捷、灵敏度高、准确性好,能够满足对鸡蛋中氟虫腈残留量的检测需要。
A gas chromatographic method(GC) for determination of fipronil residues in eggs was established. In this method,the samples were extracted with acetonitrile/water,then further cleaned up by HLB solid-phase extraction column. Good linear relationship was obtained in the concentrations of 0.000 5~0.064 0 μg/m L,while the correlation coefficient was 0.999 85. The detection limit of this method was 0.6 μg/kg and the average recoveries was 73.4%~84.2%. The relative standard derivation(RSD) was 6.1%~8.6%. The method is simple,rapid,sensitive and accurate to meet the needs of the analysis,which could be used for the detection of fipronil residues in eggs.
引文
[1]Tomlin C.The pesticide manual:A world compendium[M].11th ed.Alton:The British Crop Protection Council,1997:462-464.
[2]付晓芳,林雁飞,李晶,等.茶叶中氟虫腈残留量的检测[J].食品科学,2010,31(10):279-282.
[3]王国胜,丁宁,肖琦诗,等.食品中氟虫腈检测方法的研究[J].畜牧兽医科技信息,2018(12):36-37.
[4]张珍珍.氟虫腈的危害及其在鸡蛋中残留检测方法[J].河北农业,2018(9):43-44.
[5]赵健,朱勇,王立君,等.大白菜、甘蓝和西兰花中锐劲特残留量气相色谱分析方法的研究[J].分析试验室,2006(11):93-95.
[6]周晓冬,余兵,胡进.豆类蔬菜中氟虫腈残留分析方法的研究[J].农业环境科学学报,2007(S1):211-214.
[7]荣维广,武中平,高巍,等.氟虫腈的色谱分析方法[J].农药,2006(8):547-549.
[8]陆贻通,周培,吴银良,等.锐劲特在菜地生态系统中的残留动态研究[J].环境污染与防治,2001(5):219-221,231.
[9]曹维强,赵海田,佘永新,等.气相色谱-质谱联用对菠菜中丁烯氟虫腈残留的检测[J].分析测试学报,2009,28(9):1 096-1 099.
[10]GB/T 23204-2008,茶叶中519种农药及相关化学品残留量的测定气相色谱-质谱法[S].北京:中国标准出版社,2008.
[11]陈珊珊,丁丞,郭立新,等.气相色谱-负化学电离-质谱联用技术检测痕量氟虫腈及代谢物的漂移对池塘水和虾体的影响[J].质谱学报,2013,34(5):274-281.
[12]荣杰峰,韦航,李亦军,等.食品中氟虫腈残留量的检测方法研究进展[J].广州化工,2013,41(8):16-17,21.
[13]龚勇,朴秀英,孙丰收,等.高效液相色谱-串联质谱法检测鸡蛋中氟虫腈及其代谢物的残留[J].农药科学与管理,2018,39(3):48-52.