高效液相色谱-串联质谱法同时测定枸杞中4种农药残留
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摘要
建立了高效液相色谱-串联质谱同时检测枸杞中甲基异柳磷等4种农药残留的分析方法。样品经乙腈提取,QuEChERS净化,高效液相色谱-串联质谱测定。结果表明,在质量浓度0.01～0.5mg/L时,4种农药的质量浓度与相应的峰面积呈良好的线性关系,相关系数均大于0.99。在0.01～0.5 mg/kg添加质量分数下,4种农药的添加回收率为80.3%～102.8%,相对标准偏差(RSD)为1.8%～11.2%,定量限为0.01 mg/kg。本方法快速、简便,净化效果好,且成本低,适用于4种农药在枸杞中的残留检测。
A method for the simultaneous determination of 4 kinds of pesticide residues in wolfberry was established.The samples were extracted with acetonitrile and purified by the Qu EChERS method, and detected by HPLC-MS/MS. The results demonstrated that the concentrations of 4 kinds of pesticides had a good linear relationship with the corresponding peak area in the range of 0.01-0.5 mg/kg, and the correlation coefficients were all above 0.99. The average recoveries of 4 kinds of pesticides ranged from 80.3% to 102.8%, with the RSD of 1.8%-11.2%. The limits of quantification were all 0.01 mg/kg. The method was rapid, simple, effective, inexpensive, and suitable for the simultaneous determination of 4 kinds of pesticides in wolfberry.
A method for the simultaneous determination of 4 kinds of pesticide residues in wolfberry was established.The samples were extracted with acetonitrile and purified by the Qu EChERS method, and detected by HPLC-MS/MS. The results demonstrated that the concentrations of 4 kinds of pesticides had a good linear relationship with the corresponding peak area in the range of 0.01-0.5 mg/kg, and the correlation coefficients were all above 0.99. The average recoveries of 4 kinds of pesticides ranged from 80.3% to 102.8%, with the RSD of 1.8%-11.2%. The limits of quantification were all 0.01 mg/kg. The method was rapid, simple, effective, inexpensive, and suitable for the simultaneous determination of 4 kinds of pesticides in wolfberry.
引文
[1]李鹏,郝凤霞.气相色谱法检测宁夏枸杞中联苯菊酯残留量[J].湖北农业科学, 2012, 51(7):1453-1455.
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[3] Tang H L, Chen C, Wang S K, et al. Biochemical Analysis and Hypoglycemic Activity of a Polysaccharide Isolated from the Fruit of Lycium barbarum L.[J]. International Journal of Biological Macromolecules, 2015, 77:235-242.
[4] Manthey A L, Chiu K, So K F. Effects of Lycium barbarum on the Visual System[J]. International Review of Neurobiology, 2017, 135:1-27.
[5]李莉,江树人,潘灿平,等.分散固相萃取-气相色谱-质谱方法快速净化测定枸杞中12种农药残留[J].农药学学报, 2006, 8(4):371-374.
[6]林童,魏玉海,凤晓博,等.超高效液相色谱-串联质谱法测定枸杞中常见的5种农药残留[J].现代农药, 2015, 14(1):37-39.
[7]王晓菁,潘灿平,张艳,等.枸杞中吡虫啉、阿维菌素农药残留量的测定[J].西北农业学报, 2007, 16(2):250-252.
[8]郝凤霞,李学晴,齐瑾,等. MSPD-HPLC同时测定枸杞中3种氨基甲酸酯类农药[J].农药, 2015, 54(7):525-527.
[9]李飞飞,魏悦,张海艳,等.气相色谱法同时测定枸杞中联苯菊酯、硫丹和高效氯氟氰菊酯的残留[J].湖北农业科学, 2016, 55(1):183-185.
[10]张艳,苟金萍,程淑华,等.枸杞中有机磷和氨基甲酸酯类农药残留量的测定[J].西北农业学报, 2005, 14(2):84-86.
[11] Huang X, Xue J, Wang Y, et al. Rapid Simultaneous Determination of Organochlorine and Pyrethroid Pesticide Residues in Lycium barbarum L. Using Gas Chromatography with Electron-Capture Detector[J]. Analytical Methods, 2012, 4(4):1132-1141.
[12]郝凤霞,李雪晴,朱楠,等. GC-MS同时测定枸杞中六种有机磷农药[J].湖北农业科学, 2016, 55(12):3176-3178.
[13]林祥群,卢春霞,罗小玲,等.气相色谱-质谱法测定枸杞中28种农药残留[J].江苏农业科学, 2016, 44(1):285-289.
[14] Fu Y, Yang T, Zhao J, et al. Determination of Eight Pesticides in Lycium barbarum by LC-MS/MS and Dietary Risk Assessment[J].Food Chemistry, 2017, 218:192-198.
[15]粟有志,冯峰,刘翠平,等. QuEChERS-液相色谱-串联质谱法测定植物源食品中氟噻草胺和乙酰甲草胺残留[J].分析试验室,2017(1):81-86.
[16]周均,粟有志,李芳,等. QuEChERS-高效液相色谱-串联质谱法测定植物源性食品中噻氟隆和炔草隆残留[J].分析科学学报,2017, 33(4):535-540.
[2]曹殿洁. GC-MS检测中药枸杞中有机磷类农药残留[J].赤峰学院学报:自然科学版, 2013, 29(11):6-7.
[3] Tang H L, Chen C, Wang S K, et al. Biochemical Analysis and Hypoglycemic Activity of a Polysaccharide Isolated from the Fruit of Lycium barbarum L.[J]. International Journal of Biological Macromolecules, 2015, 77:235-242.
[4] Manthey A L, Chiu K, So K F. Effects of Lycium barbarum on the Visual System[J]. International Review of Neurobiology, 2017, 135:1-27.
[5]李莉,江树人,潘灿平,等.分散固相萃取-气相色谱-质谱方法快速净化测定枸杞中12种农药残留[J].农药学学报, 2006, 8(4):371-374.
[6]林童,魏玉海,凤晓博,等.超高效液相色谱-串联质谱法测定枸杞中常见的5种农药残留[J].现代农药, 2015, 14(1):37-39.
[7]王晓菁,潘灿平,张艳,等.枸杞中吡虫啉、阿维菌素农药残留量的测定[J].西北农业学报, 2007, 16(2):250-252.
[8]郝凤霞,李学晴,齐瑾,等. MSPD-HPLC同时测定枸杞中3种氨基甲酸酯类农药[J].农药, 2015, 54(7):525-527.
[9]李飞飞,魏悦,张海艳,等.气相色谱法同时测定枸杞中联苯菊酯、硫丹和高效氯氟氰菊酯的残留[J].湖北农业科学, 2016, 55(1):183-185.
[10]张艳,苟金萍,程淑华,等.枸杞中有机磷和氨基甲酸酯类农药残留量的测定[J].西北农业学报, 2005, 14(2):84-86.
[11] Huang X, Xue J, Wang Y, et al. Rapid Simultaneous Determination of Organochlorine and Pyrethroid Pesticide Residues in Lycium barbarum L. Using Gas Chromatography with Electron-Capture Detector[J]. Analytical Methods, 2012, 4(4):1132-1141.
[12]郝凤霞,李雪晴,朱楠,等. GC-MS同时测定枸杞中六种有机磷农药[J].湖北农业科学, 2016, 55(12):3176-3178.
[13]林祥群,卢春霞,罗小玲,等.气相色谱-质谱法测定枸杞中28种农药残留[J].江苏农业科学, 2016, 44(1):285-289.
[14] Fu Y, Yang T, Zhao J, et al. Determination of Eight Pesticides in Lycium barbarum by LC-MS/MS and Dietary Risk Assessment[J].Food Chemistry, 2017, 218:192-198.
[15]粟有志,冯峰,刘翠平,等. QuEChERS-液相色谱-串联质谱法测定植物源食品中氟噻草胺和乙酰甲草胺残留[J].分析试验室,2017(1):81-86.
[16]周均,粟有志,李芳,等. QuEChERS-高效液相色谱-串联质谱法测定植物源性食品中噻氟隆和炔草隆残留[J].分析科学学报,2017, 33(4):535-540.