固相萃取-气相色谱-火焰光度法同时测定植物性肽粉中42种有机磷农药残留
|
摘要
建立了植物性肽粉中42种有机磷农药的固相萃取-气相色谱-火焰光度检测器(SPE-GC-FPD)方法。样品用乙腈作为提取溶剂,提取液过石墨化炭黑-氨基复合柱净化,用乙腈-甲苯(体积分数为75%)洗脱,气相色谱-火焰光度检测器检测,外标法定量。在0.05和0.5 mg/kg的添加水平下,42种有机磷的平均回收率为72.8%~103.8%,相对标准偏差在2.44%~8.71%,该方法的检出限为0.005~0.020 mg/kg,定量低限为0.015~0.060 mg/kg。采用所建立方法测定了10种代表性的植物性肽粉中42种有机磷农药残留量,结果均未检出。该方法简单快捷、普及度高,适用于植物性肽粉中多种有机磷农药的分离与定量。
A method for the determination of 42 kinds of organophosphorus pesticide in plant-based peptide powder by solid-phase extraction-gas chromatography-flame photometric detector( SPE-GC-FPD) was established. The samples were extracted by acetonitrile,concentrated and purified by solid phase extracted on Pesti Carb/NH2 column,eluted with acetonitrile/toluene( volume fraction is 75%). Finally,the pesticides were determined by flame photometric detector( FPD),quantified by external standard method. The recoveries were 72. 8%-103. 8% at 2 spiked levels of 0. 05 and 0. 50 mg/kg for 42 organophosphorus pesticides,and the relative standard deviations( RSDs) were between 2. 44%-8. 71%. The limits of detections were in the range of 0. 005-0. 020 mg/kg and the limits of quantitation were in the range of 0. 015-0. 060 mg/kg. A total of 10 plant-based peptides was tested and none of these pesticides were detected. The method can be applied to determine organophosphorus pesticides in plant-based peptide powder samples due to its efficiency and simplicity.
A method for the determination of 42 kinds of organophosphorus pesticide in plant-based peptide powder by solid-phase extraction-gas chromatography-flame photometric detector( SPE-GC-FPD) was established. The samples were extracted by acetonitrile,concentrated and purified by solid phase extracted on Pesti Carb/NH2 column,eluted with acetonitrile/toluene( volume fraction is 75%). Finally,the pesticides were determined by flame photometric detector( FPD),quantified by external standard method. The recoveries were 72. 8%-103. 8% at 2 spiked levels of 0. 05 and 0. 50 mg/kg for 42 organophosphorus pesticides,and the relative standard deviations( RSDs) were between 2. 44%-8. 71%. The limits of detections were in the range of 0. 005-0. 020 mg/kg and the limits of quantitation were in the range of 0. 015-0. 060 mg/kg. A total of 10 plant-based peptides was tested and none of these pesticides were detected. The method can be applied to determine organophosphorus pesticides in plant-based peptide powder samples due to its efficiency and simplicity.
引文
[1]YANG Xiao-hong,XIA Jiang-nan,YU Zhi-jun,et al.Characterization of diverse antimicrobial peptides in skin secretions of Chungan torrent frog Amolops chunganensis[J].Peptides,2012,38(1):41-53.
[2]SARMADI B H,ISMAIL A.Antioxidative peptides from food proteins:A review[J].Peptides,2010,31(10):1 949-1 956.
[3]王桂春,吕兵.分步酶解酪蛋白制备小分子ACE抑制肽[J].食品科学,2011,32(21):152-155.
[4]王子怀,胡晓,李来好,等.肽-金属离子螯合物的研究进展[J].食品工业科技,2014,35(8):359-362.
[5]郭辉,何慧,韩樱,等.玉米肽对小鼠酒后肝脏乙醇脱氢酶活力的影响及醒酒机理[J].食品科学,2011,32(11):265-269.
[6]刘永,唐英斐,宋金凤,等.固相萃取-液相色谱-串联质谱法测定蔬菜中4种有机磷农药及其代谢产物[J].色谱,2014,32(2):140.
[7]黄晓会,沈艳琳,陈俊珺,等.GC-FPD法检测果实类中药材中有机磷农药残留[J].中华中医药杂志,2015,30(7):2 483.
[8]寇婷婷,徐昆龙,张灵枝,等.普洱茶中有机磷类农药残留的测定[J].食品科学,2010,31(12):165-168.
[9]苏建峰,钟茂生,陈晶,等.气相色谱-质谱法与气相色谱法测定茶叶及茶叶加工品中295种农药多残留[J].分析测试学报,2015,34(6):625-638.
[10]李萍萍,程景,乐渊.气相色谱-三重四极杆串联质谱法测定含硫蔬菜中46种农药残留量[J].分析测试学报,2015,34(4):421-427.
[11]文孟棠,刘媛,寇莉萍,等.大白菜中拟除虫菊酯类农药半定量ELISA免疫检测方法的建立[J].江苏农业学报,2014,30(2):411-416.
[12]张爱芝,王全林,曹丽丽,等.Qu ECHERS-超高效液相色谱-串联质谱法测定蔬菜中250种农药残留[J].色谱,2016,34(2):158-164.
[13]徐国锋,聂继云,李海飞,等.Qu ECHERS/气相色谱法测定水果中31有机磷农药残留[J].分析测试学报,2016,35(8):1 021.
[14]冯敏,李亚楠,高丽霞,等.酶联免疫吸附法在食品安全性指标检测中的研究进展[J].食品安全质量检测学报,2016,7(10):3 974.
[15]曹小丽,刘素华,刘仲,等.气相色谱-串联质谱结合Qu ECHERS方法检测蔬釆、水果中62种农药残留[J].中国卫生检验杂志,2015,25(8):1 121.
[16]叶瑞洪,苏建峰.分散固相萃取-超高效液相色谱串联质谱法测定果蔬、牛奶、植物油和动物肌肉中残留的61种有机磷农药[J].色谱,2011,29(7):621.
[17]左海根,占春瑞,伍彩花,等.气相色谱法测定大豆中24种有机磷农药的残留量[J].理化检验-化学分册,2010,46(10):1 202.
[18]贺利民,刘祥国,曾振灵.气相色谱分析农药残留的基质效应及其解决方法[J].色谱,2008,26(1):101.
[19]PAULA PAYA,MICHELANGELO ANASTASSIADE,DOROTHEA MACK,et al.Analysis of pesticide residues using the quick easy cheap effective rugged and safe(Qu ECh ERS)pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection[J].Analytical and Bioanalytical Chemistry,2007,386(6):1 697-1 714.
[20]中国合格评定国家认可中心.GB/T 27404—2008实验室质量控制规范食品理化检测[S].北京:中国标准出版社,2008.
[2]SARMADI B H,ISMAIL A.Antioxidative peptides from food proteins:A review[J].Peptides,2010,31(10):1 949-1 956.
[3]王桂春,吕兵.分步酶解酪蛋白制备小分子ACE抑制肽[J].食品科学,2011,32(21):152-155.
[4]王子怀,胡晓,李来好,等.肽-金属离子螯合物的研究进展[J].食品工业科技,2014,35(8):359-362.
[5]郭辉,何慧,韩樱,等.玉米肽对小鼠酒后肝脏乙醇脱氢酶活力的影响及醒酒机理[J].食品科学,2011,32(11):265-269.
[6]刘永,唐英斐,宋金凤,等.固相萃取-液相色谱-串联质谱法测定蔬菜中4种有机磷农药及其代谢产物[J].色谱,2014,32(2):140.
[7]黄晓会,沈艳琳,陈俊珺,等.GC-FPD法检测果实类中药材中有机磷农药残留[J].中华中医药杂志,2015,30(7):2 483.
[8]寇婷婷,徐昆龙,张灵枝,等.普洱茶中有机磷类农药残留的测定[J].食品科学,2010,31(12):165-168.
[9]苏建峰,钟茂生,陈晶,等.气相色谱-质谱法与气相色谱法测定茶叶及茶叶加工品中295种农药多残留[J].分析测试学报,2015,34(6):625-638.
[10]李萍萍,程景,乐渊.气相色谱-三重四极杆串联质谱法测定含硫蔬菜中46种农药残留量[J].分析测试学报,2015,34(4):421-427.
[11]文孟棠,刘媛,寇莉萍,等.大白菜中拟除虫菊酯类农药半定量ELISA免疫检测方法的建立[J].江苏农业学报,2014,30(2):411-416.
[12]张爱芝,王全林,曹丽丽,等.Qu ECHERS-超高效液相色谱-串联质谱法测定蔬菜中250种农药残留[J].色谱,2016,34(2):158-164.
[13]徐国锋,聂继云,李海飞,等.Qu ECHERS/气相色谱法测定水果中31有机磷农药残留[J].分析测试学报,2016,35(8):1 021.
[14]冯敏,李亚楠,高丽霞,等.酶联免疫吸附法在食品安全性指标检测中的研究进展[J].食品安全质量检测学报,2016,7(10):3 974.
[15]曹小丽,刘素华,刘仲,等.气相色谱-串联质谱结合Qu ECHERS方法检测蔬釆、水果中62种农药残留[J].中国卫生检验杂志,2015,25(8):1 121.
[16]叶瑞洪,苏建峰.分散固相萃取-超高效液相色谱串联质谱法测定果蔬、牛奶、植物油和动物肌肉中残留的61种有机磷农药[J].色谱,2011,29(7):621.
[17]左海根,占春瑞,伍彩花,等.气相色谱法测定大豆中24种有机磷农药的残留量[J].理化检验-化学分册,2010,46(10):1 202.
[18]贺利民,刘祥国,曾振灵.气相色谱分析农药残留的基质效应及其解决方法[J].色谱,2008,26(1):101.
[19]PAULA PAYA,MICHELANGELO ANASTASSIADE,DOROTHEA MACK,et al.Analysis of pesticide residues using the quick easy cheap effective rugged and safe(Qu ECh ERS)pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection[J].Analytical and Bioanalytical Chemistry,2007,386(6):1 697-1 714.
[20]中国合格评定国家认可中心.GB/T 27404—2008实验室质量控制规范食品理化检测[S].北京:中国标准出版社,2008.