水产品中有机磷农药多残留的固相萃取-气相色谱串联质谱测定
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摘要
通过比较不同的提取剂和吸附剂对水产品的净化效果和对质谱基线的影响,建立一种有效的水产品中有机磷农药多残留的气相色谱-三重四极杆串联质谱(GC-MS/MS)方法。用正己烷对样品进行提取处理,采用N-丙基二乙胺(PSA)和硅胶柱进行固相萃取,用GC-MS/MS多反应离子监测(MRM)模式测定。结果表明,在5～200μg·L-1范围内,28种有机磷农药的峰面积与对应的质量浓度间呈良好的线性关系,相关系数R2>0.996 8,方法的定量限(S/N=10)为0.2～7.9μg·kg-1,在大黄鱼中各农药的回收率为67%～99%之间,相对标准偏差(RSD)在5.3%～13.6%(n=6)之间,在南美白对虾中各农药的回收率为73%～106%之间,相对标准偏差(RSD)在4.6%～12.8%(n=6)之间。该方法较为灵敏、准确、简便,可用于检测水产品的有机磷农药残留情况。
A gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS) method for the determination of organophosphorus pesticides residues in aquatic products was established by comparing the effects of different extractants and adsorbents on the purification effect and the baseline of mass spectrometry. The sample was extracted with hexane, PSA and silica gel column were used for solid phase extraction,and GC-MS/MS MRM was used to determine the sample. The results show that there is a good linear relationship between the peak area of the 28 organophosphorus pesticides and the corresponding mass concentration in the range of 5-200 μg·L-1, the correlation coefficient R2>0.996 8, the quantitative limit(S/N=10) of the method is 0.2-7.9 μg·kg~(-1), the recovery rate of each pesticide in the large yellow croaker is 67%-99%, and the relative standard deviation(RSD) is in 5.3%-13.6%(n=6) the recovery rate of pesticides in Penaeus vannamei was between 73%-106%, and the relative standard deviation(RSD) was between 4.6%-12.8%(n=6). The method is sensitive, accurate and simple, and can be used to detect organophosphorus pesticide residues in aquatic products.
A gas chromatography-triple quadrupole tandem mass spectrometry(GC-MS/MS) method for the determination of organophosphorus pesticides residues in aquatic products was established by comparing the effects of different extractants and adsorbents on the purification effect and the baseline of mass spectrometry. The sample was extracted with hexane, PSA and silica gel column were used for solid phase extraction,and GC-MS/MS MRM was used to determine the sample. The results show that there is a good linear relationship between the peak area of the 28 organophosphorus pesticides and the corresponding mass concentration in the range of 5-200 μg·L-1, the correlation coefficient R2>0.996 8, the quantitative limit(S/N=10) of the method is 0.2-7.9 μg·kg~(-1), the recovery rate of each pesticide in the large yellow croaker is 67%-99%, and the relative standard deviation(RSD) is in 5.3%-13.6%(n=6) the recovery rate of pesticides in Penaeus vannamei was between 73%-106%, and the relative standard deviation(RSD) was between 4.6%-12.8%(n=6). The method is sensitive, accurate and simple, and can be used to detect organophosphorus pesticide residues in aquatic products.
引文
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[7]田甜,赵德恩,梁登雲,等.分散固相萃取-气相色谱-质谱法测定果蔬汁中6种有机磷农药的残留量[J].食品安全质量检测学报, 2018, 9(6):1 388-1 394.
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[10]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):139-144.
[11]王连珠,周昱,陈泳,等. QuEChERS样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估[J].色谱, 2012, 30(2):146-153.
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[16] HAMMOCK B D, MUMMA R O. Potential of Immunochemical Technology for Pesticide Analysis[C]//HARVEY J Jr, ZWEIG G. Pesticide Analytical Methodology, Washimgton DC:American Chemica Society, 1980:321-352.
[17] CLEGG B S, STEPHENSON G R, HALL J C. DEVELOPMENT OF AN ENZYME-LINKED IMMUNOSORBENT ASSAY FOR THE DETECTION OF GLYPHOSAT E[J]. JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, 1999, 47(12):5031-5037.
[18]王雪荣,刘振波,贾风燕,等.有机磷药物在水产品中的存在状态研究及其分析应用[J].化学学报, 2011, 69(20):2 505-2510.
[19]沈丹玉,袁新跃,刘毅华,等.分散固相净化与气相色谱测定竹笋中21种农药残留[J].食品科学, 2017, 38(16):268-273.
[20] NY/T 788-2018农作物中农药残留试验准则[S].北京:中国农业出版社, 2018.
[2]廖和菁,张雪春,胡礼渊,等.气相色谱法同时测定茶叶中10种有机磷农药残留[J].中国食品卫生杂志, 2015, 27(1):41-44.
[3]黄倩,何蔓,陈贝贝,等.磁固相萃取-气相色谱-火焰光度检测联用测定果汁中的有机磷农药[J].色谱, 2014, 32(10):1 131-1 137.
[4]胡业琴,郗存显,曹淑瑞,等.介孔氧化铝净化-气相色谱法同时测定蔬菜、水果及茶叶中16种有机磷农药残留[J].色谱,2014, 32(7):784-788.
[5]马妍,陈曦,沈葹,等.浸入式固相微萃取-气相色谱-质谱法测定中草药液体保健食品中25种有机磷农药残留[J].卫生研究, 2018, 47(3):446-452.
[6]于洪,许秀艳,许人骥,等.微波萃取-气相色谱/串联质谱测定贝中有机磷农药[J].中国测试, 2018, 44(4):64-68.
[7]田甜,赵德恩,梁登雲,等.分散固相萃取-气相色谱-质谱法测定果蔬汁中6种有机磷农药的残留量[J].食品安全质量检测学报, 2018, 9(6):1 388-1 394.
[8]陈军华.高效液相色谱法在中草药黄酮类化合物和水中有机磷农药分析中的应用研究[D].重庆:西南大学, 2016.
[9]魏天龙.高效液相色谱法同时测定生活饮用水中七种有机磷农药残留研究[D].兰州:西北师范大学, 2013.
[10]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):139-144.
[11]王连珠,周昱,陈泳,等. QuEChERS样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估[J].色谱, 2012, 30(2):146-153.
[12]余骏.气相色谱法测定水产品中有机磷农药残留[A].中国化学会色谱专业委员会、中国色谱学会、中国科学院大连化学物理研究所.第十五次全国色谱学术报告会文集(上册)[C].中国化学会色谱专业委员会、中国色谱学会、中国科学院大连化学物理研究所:中国化学会, 2005:2.
[13]张云,李耀平,李敏新,等.液相色谱-串联质谱法测定水产品中7种有机磷类农药残留物[J].分析试验室, 2009, 28(S1):191-194.
[14]牛佳钰,肖纯凌.有机磷农药的残留危害及检测方法研究[J].安徽农业科学, 2016, 44(16):87-89.
[15] ERCEGOVICH C D, VALLEJO R P, GETTIG R R, et al. Development of a radioimmunoassay for parathion[J]. Journal of Agricultural and Food Chemistry, 1981, 29(3):559-603.
[16] HAMMOCK B D, MUMMA R O. Potential of Immunochemical Technology for Pesticide Analysis[C]//HARVEY J Jr, ZWEIG G. Pesticide Analytical Methodology, Washimgton DC:American Chemica Society, 1980:321-352.
[17] CLEGG B S, STEPHENSON G R, HALL J C. DEVELOPMENT OF AN ENZYME-LINKED IMMUNOSORBENT ASSAY FOR THE DETECTION OF GLYPHOSAT E[J]. JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY, 1999, 47(12):5031-5037.
[18]王雪荣,刘振波,贾风燕,等.有机磷药物在水产品中的存在状态研究及其分析应用[J].化学学报, 2011, 69(20):2 505-2510.
[19]沈丹玉,袁新跃,刘毅华,等.分散固相净化与气相色谱测定竹笋中21种农药残留[J].食品科学, 2017, 38(16):268-273.
[20] NY/T 788-2018农作物中农药残留试验准则[S].北京:中国农业出版社, 2018.