超高效液相色谱串联质谱法快速定量检测鸡蛋中的氟虫腈及其三种代谢物
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摘要
基于超高效液相色谱串联质谱技术,本文建立了一种鸡蛋中氟虫腈及其三种代谢物(氟甲腈、氟虫腈砜、氟虫腈亚砜)的快速检测方法。鸡蛋去壳后匀浆,经乙腈提取后盐析,上清液采用UPLC-MS/MS-ESI负离子多反应检测模式进行分析测定。结果表明,氟虫腈及三种代谢物在0.1-20.0ng/mL范围内线性良好,检出限为0.15～0.35ug/kg,定量限为0.55～0.7ug/kg,平均加标回收率在95.00%～105.58%之间,相对标准偏差在1.10%～5.01%之间。该方法便捷快速且准确定量,可应用于实际样品检测中。
Based on ultra performance liquid chromatography-tandem mass spectrometry(LC-MS),a rapid detection method for fipronil and its three metabolites(fipronil desulfinyl,fipronil sulfone,fipronil sulfide) in eggs was established.The shell of egg was removed,then the eggs were homogenized,extracted by acetonitrile,and then subjected to salting out.The supernatant was analyzed by LC-MS with multi-reaction mode in negative ion mode.The results showed that fipronil and three metabolites were linear in the range of 0.1-20.0 ng/mL,the detection limit was 0.15～0.35 ug/kg and the limit of quantification was 0.55～0.7 ug/kg.The average spiked recovery rate was from 95.00% to 105.58%,the relative standard deviation was between 1.10% and 5.01%.This method is rapid and accurate,which can be applied to actual sample detection.
Based on ultra performance liquid chromatography-tandem mass spectrometry(LC-MS),a rapid detection method for fipronil and its three metabolites(fipronil desulfinyl,fipronil sulfone,fipronil sulfide) in eggs was established.The shell of egg was removed,then the eggs were homogenized,extracted by acetonitrile,and then subjected to salting out.The supernatant was analyzed by LC-MS with multi-reaction mode in negative ion mode.The results showed that fipronil and three metabolites were linear in the range of 0.1-20.0 ng/mL,the detection limit was 0.15～0.35 ug/kg and the limit of quantification was 0.55～0.7 ug/kg.The average spiked recovery rate was from 95.00% to 105.58%,the relative standard deviation was between 1.10% and 5.01%.This method is rapid and accurate,which can be applied to actual sample detection.
引文
[1] 胡骁飞,魏凤仙,李向力,等.氟虫腈的危害及检测技术研究进展[J].食品安全质量检测学报,2018,9(06):1226-1233.
[2] 宁霄,金绍明,高文超,等.QuEChERS-超高效液相色谱-串联质谱法测定动物源性食品中氟虫腈及其代谢物残留[J].分析化学,2018,46(08):1297-1305.
[3] 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.
[4] 夏义平,尹啸冰,林肖惠,田阳光.QuEChERS-固相萃取-高效液相色谱-串联质谱法快速测定鸡蛋和鸡肉中氟虫腈及其代谢产物[J].中国食品卫生杂志,2018,30(04):395-400.
[5] 余文婷,杨亚宣,雷春华,曾凯.鸡蛋中氟虫腈及其代谢产物的快速测定方法研究[J].江西农业大学学报,2018,40(04):850-855+865.
[6] 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.
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[10] 崔相勇,穆姣姣,王岩松,等.液相色谱-串联质谱法测定鸡蛋中氟虫腈及其3种代谢物的含量[J].理化检验(化学分册),2018,54(05):601-605.
[11]v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.
[12]v周鹏,黄芊,欧阳立群,等.稳定同位素稀释超高效液相色谱-串联质谱法测定饲料中氟虫腈及其代谢物[J].色谱,2018,36(07):629-633.
[13] 金绍明,宁霄,高文超,曹进.烹饪方法对鸡蛋及鸡肉中氟虫腈及其代谢物残留量的影响[J].肉类研究,2018,32(06):40-43.
[14] ZhangM Y,Bian K,Zhou T,et al.Determination of residual fipronil in chicken egg and muscleby LC-MS/MS[J].Journal of Chromatography B,2016,1014(1):31-36.
[15] 时逸吟,李优,伊雄海,等.液相色谱-串联质谱法测定蛋及蛋制品中氟虫腈及其代谢物的残留量[J].检验检疫学刊,2017,27(05):1-7.
[16] 食品中农药最大残留限量.中华人民共和国国家标准.GB 2763-2016.
[17] 农业部.中华人民共和国农业部公告第1157 号公告,[2009-02-08].
[18] 曾凯,余文婷,杨亚宣,罗明标.气相色谱-三重四极杆质谱法测定鸡蛋中氟虫氰及其代谢残留[J].分析试验室,2018,37(06):677-680.
[19] 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.
[20] Duhan A,Kunari B,Duhan S.Determination of residual of fipronil and its metabolites in cauliflower by using gas chromatography-tandem mass spectrometry[J].Bulletin of Environmental Contamination and Toxicology,2015,94(2):260-266.
[21] 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.
[22] Subrata B,Mondal R,Mukherjee A,et al.Simultaneous determination and risk assessment of fipronil and its metabolites in sugarcane,using GC-ECD and confirmation by GC-MS/MS[J].Food Chemistry,2019,272(30):559-567.
[23] 张立佳,白艳梅,吕志勇,等.超高效液相色谱-串联质谱法测定全蛋粉、蛋黄粉及乳制品中氟虫腈及其代谢物[J].乳业科学与技术,2018,41(04):34-38.
[24] 郝杰,邵瑞婷,姜洁,贺小蔚.QuEChERS-超高效液相色谱-串联质谱法测定鸡蛋、鸡肉中氟虫腈及其代谢物残留[J].食品科学,2019(02):318-323.
[25] Zheng W J,Park J A,El-Aty AM,et al.Development and validation of modified QuEChERS method coupled with LC-MS/MS for simultaneous determination of cymiazole,fipronil,coumaphos,fluvalinate,amitraz,and its metabolite in various types of honey and royal jelly[J].Journal of Chromatography B,2018,1072(1):60-69.
[2] 宁霄,金绍明,高文超,等.QuEChERS-超高效液相色谱-串联质谱法测定动物源性食品中氟虫腈及其代谢物残留[J].分析化学,2018,46(08):1297-1305.
[3] 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.
[4] 夏义平,尹啸冰,林肖惠,田阳光.QuEChERS-固相萃取-高效液相色谱-串联质谱法快速测定鸡蛋和鸡肉中氟虫腈及其代谢产物[J].中国食品卫生杂志,2018,30(04):395-400.
[5] 余文婷,杨亚宣,雷春华,曾凯.鸡蛋中氟虫腈及其代谢产物的快速测定方法研究[J].江西农业大学学报,2018,40(04):850-855+865.
[6] 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.
[7] Zuzana,JankaB,tefan,et al.Fipronil causes toxicity in mouse preimplantation embryos[J].Toxicology,2018,410(1):214-221.
[8] 柏再苏.锐劲特及其代谢和光降解产物的毒性综述[J].现代农药,2003,(2):1-3.
[9] 柳菡,龚玉霞,王绳芸,等.气相色谱-串联质谱法测定蛋和蛋制品中氟虫腈及其代谢物残留量[J].质谱学报,2018.
[10] 崔相勇,穆姣姣,王岩松,等.液相色谱-串联质谱法测定鸡蛋中氟虫腈及其3种代谢物的含量[J].理化检验(化学分册),2018,54(05):601-605.
[11]v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.
[12]v周鹏,黄芊,欧阳立群,等.稳定同位素稀释超高效液相色谱-串联质谱法测定饲料中氟虫腈及其代谢物[J].色谱,2018,36(07):629-633.
[13] 金绍明,宁霄,高文超,曹进.烹饪方法对鸡蛋及鸡肉中氟虫腈及其代谢物残留量的影响[J].肉类研究,2018,32(06):40-43.
[14] ZhangM Y,Bian K,Zhou T,et al.Determination of residual fipronil in chicken egg and muscleby LC-MS/MS[J].Journal of Chromatography B,2016,1014(1):31-36.
[15] 时逸吟,李优,伊雄海,等.液相色谱-串联质谱法测定蛋及蛋制品中氟虫腈及其代谢物的残留量[J].检验检疫学刊,2017,27(05):1-7.
[16] 食品中农药最大残留限量.中华人民共和国国家标准.GB 2763-2016.
[17] 农业部.中华人民共和国农业部公告第1157 号公告,[2009-02-08].
[18] 曾凯,余文婷,杨亚宣,罗明标.气相色谱-三重四极杆质谱法测定鸡蛋中氟虫氰及其代谢残留[J].分析试验室,2018,37(06):677-680.
[19] 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.
[20] Duhan A,Kunari B,Duhan S.Determination of residual of fipronil and its metabolites in cauliflower by using gas chromatography-tandem mass spectrometry[J].Bulletin of Environmental Contamination and Toxicology,2015,94(2):260-266.
[21] 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.
[22] Subrata B,Mondal R,Mukherjee A,et al.Simultaneous determination and risk assessment of fipronil and its metabolites in sugarcane,using GC-ECD and confirmation by GC-MS/MS[J].Food Chemistry,2019,272(30):559-567.
[23] 张立佳,白艳梅,吕志勇,等.超高效液相色谱-串联质谱法测定全蛋粉、蛋黄粉及乳制品中氟虫腈及其代谢物[J].乳业科学与技术,2018,41(04):34-38.
[24] 郝杰,邵瑞婷,姜洁,贺小蔚.QuEChERS-超高效液相色谱-串联质谱法测定鸡蛋、鸡肉中氟虫腈及其代谢物残留[J].食品科学,2019(02):318-323.
[25] Zheng W J,Park J A,El-Aty AM,et al.Development and validation of modified QuEChERS method coupled with LC-MS/MS for simultaneous determination of cymiazole,fipronil,coumaphos,fluvalinate,amitraz,and its metabolite in various types of honey and royal jelly[J].Journal of Chromatography B,2018,1072(1):60-69.