利用多功能针式过滤器快速检测油菜和苹果中68种农药及代谢物残留
|
摘要
针对国家农产品质量安全例行监测涉及的68种农药及代谢物,采用基于QuEChERS方法的多功能针式过滤器快速净化,建立了油菜和苹果中68种农药及11种代谢物的多残留快速检测方法,其中48种农药及8种代谢物采用液相色谱-串联质谱(LC-MS/MS), 20种农药及3种代谢物采用气相色谱-串联质谱(GC-MS/MS)进行检测分析。结果表明,目标物在0.01～0.2 mg/L范围内线性关系良好,相关系数为0.990 5～0.999 9。在0.01～0.2 mg/kg的添加水平下,油菜的回收率为60.3%～119%,相对标准偏差为0.58%～19.4%(n=5);苹果的回收率为60.5%～118%,相对标准偏差为0.71%～19.2%(n=5)。方法检出限为0.005～0.01 mg/kg,定量限为0.01～0.05 mg/kg。将本方法应用于实际样品检测,发现油菜中虫螨腈、吡虫啉、啶虫脒、氯氰菊酯、腐霉利有检出,残留量为0.012～0.21 mg/kg;苹果中戊唑醇、氯氟氰菊酯、氯氰菊酯、腐霉利、联苯菊酯有检出,残留量为0.01～0.19 mg/kg,表明所建立的方法具有良好的实用性。
引文
[1]中华人民共和国农业部.NYT 761-2008蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定[S].北京:中国农业出版社,2008.
[2]中华人民共和国卫生部,中国国家标准化管理委员会.GBT5009.147-2003植物性食品中除虫脲的测定[S].北京:中国标准出版社,2003.
[3]中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部,国家食品药品监督管理总局.GB23200.8-2016水果和蔬菜中500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,2016.
[4]中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部,国家食品药品监督管理总局.GB23200.19-2016水果和蔬菜中阿维菌素残留量的测定液相色谱法[S].北京:中国标准出版社,2016.
[5]Anastassiades M,Lehotay S J,Stajnbaher D,et al.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and"dispersive solid-phase extraction"for the determination of pesticide residues in produce[J].Journal of AOAC International,2003,86(2):412-431.
[6]Anastassiades M,Ma?tovskáK,Lehotay S J.Evaluation of analyte protectants to improve gas chromatographic analysis of pesticides[J].Journal of Chromatography A,2003,1015(1-2):163-184.
[7]Lehotay S J,Mastovska K,Lightfield A R.Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables[J].Journal of AOACInternational,2005,88(2):615-629.
[8]Hu M,Qiu J,Zhang H,et al.Method Development and Validation of Indaziflam and Its Five Metabolites in Soil,Water,and Fruits by Modified QuEChERS and UHPLC-MS/MS[J].Journal of Agricultural and Food Chemistry,2018,66(39):10 300-10 308.
[9]Koesukwiwat U,Lehotay S J,Miao S,et al.High throughput analysis of 150 pesticides in fruits and vegetables using QuEChERS and low-pressure gas chromatography-time-of-flight mass spectrometry[J].Journal of Chromatography A,2010,1 217(43):6 692-6 703.
[10]Lehotay S J,Son K A,Kwon H,et al.Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables[J].Journal of Chromatography A,2010,1 217(16):2 548-2 560.
[11]王昕璐,贾琪,许彦阳,等.QuEChERS-超高效液相色谱-串联质谱法同时测定草莓中甲基硫菌灵、多菌灵和乙嘧酚残留[J].农药学学报,2017,19(5):603-608.
[12]张婷丽,楼芝英,胡岗,等.QuEChERS-HPLC同时测定蔬果中残留氨基甲酸酯类和苯甲酰脲类农药[J].上海师范大学学报(自然科学版),2018,47(4):420-427.
[13]秦美玲,柴爽爽,马有宁,等.基于QuEChERS-液相色谱-串联质谱法测定稻米中嘧草醚和双草醚残留[J].色谱,2017,35(7):719-723.
[14]孙小龙,徐怀德,安全,等.QuEChERS气相色谱联用法检测马铃薯中4种拟除虫菊酯类农药残留及基质效应的影响[J].食品安全质量检测学报,2018,9(11):2 621-2 626.
[15]张苗苗,王素雅,鞠兴荣,等.基于QuEChERS与UPLC-Triple-TOF-MS相结合的水稻中溴氰菊酯的检测[J].食品科技,2017,48(8):314-318.
[16]刘永涛,余琳雪,王桢月,等.改良的QuEChERS结合高效液相色谱-串联质谱同时测定水产品中7种阿维菌素类药物残留[J].色谱,2017,35(12):1276-1285.
[17]张小刚,王霞,戴春风,等.QuEChERS-超高效液相色谱-串联质谱法测定牛奶中6种头孢菌素类抗生素残留[J].色谱,2018,36(4):345-350.
[18]Whelan M,Kinsella B,Furey A,et al.Determination of anthelmintic drug residues in milk using ultra high performance liquid chromatography-tandem mass spectrometry with rapid polarity switching[J].Journal of Chromatography A,2010,1 217(27):4 612-4 622.!!!!!!!!!!!!!!!!!!!!!!
[2]中华人民共和国卫生部,中国国家标准化管理委员会.GBT5009.147-2003植物性食品中除虫脲的测定[S].北京:中国标准出版社,2003.
[3]中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部,国家食品药品监督管理总局.GB23200.8-2016水果和蔬菜中500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,2016.
[4]中华人民共和国国家卫生和计划生育委员会,中华人民共和国农业部,国家食品药品监督管理总局.GB23200.19-2016水果和蔬菜中阿维菌素残留量的测定液相色谱法[S].北京:中国标准出版社,2016.
[5]Anastassiades M,Lehotay S J,Stajnbaher D,et al.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and"dispersive solid-phase extraction"for the determination of pesticide residues in produce[J].Journal of AOAC International,2003,86(2):412-431.
[6]Anastassiades M,Ma?tovskáK,Lehotay S J.Evaluation of analyte protectants to improve gas chromatographic analysis of pesticides[J].Journal of Chromatography A,2003,1015(1-2):163-184.
[7]Lehotay S J,Mastovska K,Lightfield A R.Use of buffering and other means to improve results of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables[J].Journal of AOACInternational,2005,88(2):615-629.
[8]Hu M,Qiu J,Zhang H,et al.Method Development and Validation of Indaziflam and Its Five Metabolites in Soil,Water,and Fruits by Modified QuEChERS and UHPLC-MS/MS[J].Journal of Agricultural and Food Chemistry,2018,66(39):10 300-10 308.
[9]Koesukwiwat U,Lehotay S J,Miao S,et al.High throughput analysis of 150 pesticides in fruits and vegetables using QuEChERS and low-pressure gas chromatography-time-of-flight mass spectrometry[J].Journal of Chromatography A,2010,1 217(43):6 692-6 703.
[10]Lehotay S J,Son K A,Kwon H,et al.Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables[J].Journal of Chromatography A,2010,1 217(16):2 548-2 560.
[11]王昕璐,贾琪,许彦阳,等.QuEChERS-超高效液相色谱-串联质谱法同时测定草莓中甲基硫菌灵、多菌灵和乙嘧酚残留[J].农药学学报,2017,19(5):603-608.
[12]张婷丽,楼芝英,胡岗,等.QuEChERS-HPLC同时测定蔬果中残留氨基甲酸酯类和苯甲酰脲类农药[J].上海师范大学学报(自然科学版),2018,47(4):420-427.
[13]秦美玲,柴爽爽,马有宁,等.基于QuEChERS-液相色谱-串联质谱法测定稻米中嘧草醚和双草醚残留[J].色谱,2017,35(7):719-723.
[14]孙小龙,徐怀德,安全,等.QuEChERS气相色谱联用法检测马铃薯中4种拟除虫菊酯类农药残留及基质效应的影响[J].食品安全质量检测学报,2018,9(11):2 621-2 626.
[15]张苗苗,王素雅,鞠兴荣,等.基于QuEChERS与UPLC-Triple-TOF-MS相结合的水稻中溴氰菊酯的检测[J].食品科技,2017,48(8):314-318.
[16]刘永涛,余琳雪,王桢月,等.改良的QuEChERS结合高效液相色谱-串联质谱同时测定水产品中7种阿维菌素类药物残留[J].色谱,2017,35(12):1276-1285.
[17]张小刚,王霞,戴春风,等.QuEChERS-超高效液相色谱-串联质谱法测定牛奶中6种头孢菌素类抗生素残留[J].色谱,2018,36(4):345-350.
[18]Whelan M,Kinsella B,Furey A,et al.Determination of anthelmintic drug residues in milk using ultra high performance liquid chromatography-tandem mass spectrometry with rapid polarity switching[J].Journal of Chromatography A,2010,1 217(27):4 612-4 622.!!!!!!!!!!!!!!!!!!!!!!