基于快速溶剂萃取的在线固相萃取-气质法测定鸡蛋中氟虫腈及其代谢物
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摘要
建立了鸡蛋中氟虫腈及其代谢物集提取和净化为一体的快速溶剂萃取-在线净化检测方法。样品经硅藻土分散后,装入底部有混合均匀的吸附净化剂和硅藻土的萃取池中,以乙腈为溶剂用APLE-3500萃取并同时完成净化,提取液经氮吹浓缩近干,乙腈定容至0.5mL,0.45μm有机滤膜过滤,GC-MS测定,内标法定量。该方法在0.02～1.00μg/mL范围内呈现良好的线性关系,相关系数(r)均不小于0.999,在0.025、0.05、0.1μg/g 3个浓度添加水平下氟虫腈及其代谢物的回收率为82.5%～115.7%,相对标准偏差(RSD)为1.0%～5.6%,检出限为3～7μg/kg(S/N=3),定量限为9～20μg/kg(S/N=10)。该方法自动化程度高,提取效率高,精密度好,简单,快捷,适用于鸡蛋中氟虫腈及其代谢物残留量的检测。
The extracts were concentrated by nitrogen blowing to 0.5 mL,filtered with 0.45μm organic membrane,and determined by GC-MS.Internal standard method was used for quantitative analysis.The fipronil and its metabolite showed a good linearity in the concentration range of 0.02—1μg/mL and the correlation coefficients(r)were higher than 0.999.The average recoveries were within 82.5%—115.7% at the 3 spiked levels of 0.025,0.05 and 0.1μg/g,with the relative standard deviations(RSDs)of 1.0%—5.6%.The limits of detection(LOD)(S/N=3)were in the range of 3—7μg/kg and the limits of quantification(LOQ)(S/N=10)were within 9—20μg/kg.The method is suitable for the determination of fipronil and its metabolite residues in eggs.
The extracts were concentrated by nitrogen blowing to 0.5 mL,filtered with 0.45μm organic membrane,and determined by GC-MS.Internal standard method was used for quantitative analysis.The fipronil and its metabolite showed a good linearity in the concentration range of 0.02—1μg/mL and the correlation coefficients(r)were higher than 0.999.The average recoveries were within 82.5%—115.7% at the 3 spiked levels of 0.025,0.05 and 0.1μg/g,with the relative standard deviations(RSDs)of 1.0%—5.6%.The limits of detection(LOD)(S/N=3)were in the range of 3—7μg/kg and the limits of quantification(LOQ)(S/N=10)were within 9—20μg/kg.The method is suitable for the determination of fipronil and its metabolite residues in eggs.
引文
[1]林涛,樊建麟,杨东顺,等.固相萃取-超高效液相色谱-串联质谱法测定普洱茶中氟虫腈及其类似物残留[J].农药,2015,54(11):814-817.
[2]成婧,王美玲,朱绍华,等.固相萃取-高效液相色谱-串联质谱法测定茶叶中啶虫脒、吡虫啉和氟虫腈残留量[J].食品安全质量检测学报,2016,7(01):131-137.
[3]覃玲,王生,蔡雅清.固相萃取-气质联用法测定蔬菜中氟虫腈和溴虫腈残留[J].中国卫生检验杂志,2017,27(09):1247-1249.
[4]胡贵祥,夏祥,朱惠芳.QuChERS在线凝胶色谱-气相色谱/质谱联用法测定水果蔬菜中氟虫腈农药残留[J].化学试剂,2017,39(05):509-512.
[5]白宝清,李美萍,张生万.QuEChERS-DLLME-高效液相色谱法测定蔬菜中溴虫腈和氟虫腈残留[J].食品科学,2014,35(24):254-258.
[6]邓武剑,吴卫东,赵旭,等.气相色谱-三重四极杆质谱法快速检测鸡蛋中氟虫腈及其代谢物[J].色谱,2018,36(06):547-551.
[7]刘璇.气相色谱-质谱法测定鸡蛋中氟虫腈的3种前处理方法比较[J].中国卫生检验杂志,2018,28(11):1303-1305.
[8]王艳丽,陈克云,梁秀清,等.分散固相萃取/气相色谱质谱法测定动物源性食品中的氟虫腈及其代谢物[J].分析测试学报,2018,37(04):440-445.
[9]叶倩,邓义才,路大海,等.气相色谱法测定蔬菜水果中氟虫腈等6种农药残留[J].农药,2016,55(01):51-54.
[10]田丽,王彩霞,胡佳薇,等.气相色谱-电子捕获法和气相色谱-质谱法测定水果中氟虫腈残留[J].中国卫生检验杂志,2016,26(14):1997-1999.
[11]陈沙,朱作为,黄宗兰,等.气相色谱三重四极杆串联质谱法测定鸡蛋和鸡肉中氟虫腈及其代谢物残留量的研究[J].食品安全质量检测学报,2018,9(06):1284-1289.
[12]张爱芝,李湘江,王志强,等.超高效液相色谱-串联质谱法快速测定鸡蛋中氟虫腈及其代谢物残留[J].色谱,2018,36(08):745-751.
[2]成婧,王美玲,朱绍华,等.固相萃取-高效液相色谱-串联质谱法测定茶叶中啶虫脒、吡虫啉和氟虫腈残留量[J].食品安全质量检测学报,2016,7(01):131-137.
[3]覃玲,王生,蔡雅清.固相萃取-气质联用法测定蔬菜中氟虫腈和溴虫腈残留[J].中国卫生检验杂志,2017,27(09):1247-1249.
[4]胡贵祥,夏祥,朱惠芳.QuChERS在线凝胶色谱-气相色谱/质谱联用法测定水果蔬菜中氟虫腈农药残留[J].化学试剂,2017,39(05):509-512.
[5]白宝清,李美萍,张生万.QuEChERS-DLLME-高效液相色谱法测定蔬菜中溴虫腈和氟虫腈残留[J].食品科学,2014,35(24):254-258.
[6]邓武剑,吴卫东,赵旭,等.气相色谱-三重四极杆质谱法快速检测鸡蛋中氟虫腈及其代谢物[J].色谱,2018,36(06):547-551.
[7]刘璇.气相色谱-质谱法测定鸡蛋中氟虫腈的3种前处理方法比较[J].中国卫生检验杂志,2018,28(11):1303-1305.
[8]王艳丽,陈克云,梁秀清,等.分散固相萃取/气相色谱质谱法测定动物源性食品中的氟虫腈及其代谢物[J].分析测试学报,2018,37(04):440-445.
[9]叶倩,邓义才,路大海,等.气相色谱法测定蔬菜水果中氟虫腈等6种农药残留[J].农药,2016,55(01):51-54.
[10]田丽,王彩霞,胡佳薇,等.气相色谱-电子捕获法和气相色谱-质谱法测定水果中氟虫腈残留[J].中国卫生检验杂志,2016,26(14):1997-1999.
[11]陈沙,朱作为,黄宗兰,等.气相色谱三重四极杆串联质谱法测定鸡蛋和鸡肉中氟虫腈及其代谢物残留量的研究[J].食品安全质量检测学报,2018,9(06):1284-1289.
[12]张爱芝,李湘江,王志强,等.超高效液相色谱-串联质谱法快速测定鸡蛋中氟虫腈及其代谢物残留[J].色谱,2018,36(08):745-751.