气相色谱-串联质谱法同时测定花生中97种农药
|
摘要
采用气相色谱-串联质谱法(GC-MS/MS)测定花生中97种农药。花生样品加水浸润后以0.1%乙酸乙腈为提取溶剂,超声波辅助萃取,采用改进的Qu ECh ERS法净化,气相色谱在选择反应扫描模式下测定。97种农药在6.25～200μg/L浓度范围内线性良好,线性相关系数均大于0.99,在10、20、50μg/kg 3个浓度水平下平均添加回收率在73%～120%,相对标准偏差小于17.4%(n=6)。该方法适用于花生中多种农药残留快速定量分析。
Gas chromatography-tandem mass spectrometry(GC-MS/MS) was used to determine 97 kinds of agrochemicals in peanuts. The peanut samples were soaked with water and extracted with0.1% acetonitrile acetate as solvent. The samples were purified by improved QuEChERS method,and analyzed by GC-MS/MS in selective reaction monitor mode. The calibration curves showed good linearity in the range of 6.25～200 μg/L with the correlation coefficients more than 0.99. The average recoveries of peanut were 73%～120% when the concentrations were 10, 20, 50 μg/kg, and relative standard deviations(n=6) were less than 17.4%. The method was suitable for quantitative analysis of multi-pesticide residues in peanut.
Gas chromatography-tandem mass spectrometry(GC-MS/MS) was used to determine 97 kinds of agrochemicals in peanuts. The peanut samples were soaked with water and extracted with0.1% acetonitrile acetate as solvent. The samples were purified by improved QuEChERS method,and analyzed by GC-MS/MS in selective reaction monitor mode. The calibration curves showed good linearity in the range of 6.25～200 μg/L with the correlation coefficients more than 0.99. The average recoveries of peanut were 73%～120% when the concentrations were 10, 20, 50 μg/kg, and relative standard deviations(n=6) were less than 17.4%. The method was suitable for quantitative analysis of multi-pesticide residues in peanut.
引文
[1]汤松,禹山林,廖伯寿,等.我国花生产业现状、存在问题及发展对策[J].花生学报,2010,39(3):35-38.
[2]刘若微,姚晗珺,董国堃,等.我国输日花生农残超标问题分析[J].花生学报,2007,36(4):7-11.
[3]丁小霞,李培武,周海燕,等.花生农药最大残留限量标准比对研究[J].中国油料作物学报,2011,33(5):527-531.
[4]高蓉,赵人琤,杨俊,等.高效液相色谱法测定多菌灵在油菜籽中的残留量[J].南京医科大学学报(自然科学版),2004,24(4):425-426.
[5]庞帅,丁小霞,李培武,等.HPLC-MS/MS法测定花生中5种常用农药残留量[J].中国油料作物学报,2015,37(2):246-249.
[6]孙慧,侯志广,钱永盛,等.大豆中戊唑醇的气相色谱分析方法研究[J].安徽农业科学,2011,39(15):9029-9030.
[7]陈树兵,钟莺莺,贺小雨,等.高效液相色谱-电喷雾电离串联质谱法同时测定大豆中167种农药残留[J].分析测试学报,2014,33(5):499-505.
[8]朱臻怡,冯民,何健,等.固相萃取-气相色谱法同时测定花生中18种有机氯农药残留[J].化学分析计量,2010,19(1):19-22.
[9]贝峰,崔淑华,李杰,等.MSPD/GPC-GC-NCI/MS法测定花生及其制品中68种菊酯类农药残留方法的研究[J].分析测试学报,2012,31(s1):1-7.
[10]王明泰,牟峻,吴剑,等.GC-MS法测定粮谷及油料中55种有机磷农药残留量[J].分析试验室,2006,25(11):110-117.
[11]KOESUKWIWAT U,LEHOTAY S J,MASTOVSKA K,et al.Extension of the QuEChERS method for pesticide residues in cereals to flaxseeds,peanuts,and doughs[J].Journal of Agricultural&Food Chemistry,2010,58:5950-5958.
[12]宫兆晶,李培武,张文,等.基质固相分散-气相色谱法测定油菜籽中多种有机磷农药残留[J].中国油料作物学报,2007,29(3):333-338.
[13]胡敏,李二虎,吴兵兵,等.气相色谱法测定大豆中氟乐灵、甲草胺和乙草胺农药残留[J].现代农药,2006,5(6):27-28.
[14]LI Z,LI Y,LIU X,et al.Multiresidue analysis of 58 pesticides in bean products by disposable pipet extraction(DPX)cleanup and gas chromatography-mass spectrometry determination[J].Journal of Agricultural and Food Chemistry,2012,60(19):4788-4798.
[15]LI N,WANG Z,ZHANG L,et al.Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction of herbicides in peanuts[J].Talanta,2014,128:345-353.
[2]刘若微,姚晗珺,董国堃,等.我国输日花生农残超标问题分析[J].花生学报,2007,36(4):7-11.
[3]丁小霞,李培武,周海燕,等.花生农药最大残留限量标准比对研究[J].中国油料作物学报,2011,33(5):527-531.
[4]高蓉,赵人琤,杨俊,等.高效液相色谱法测定多菌灵在油菜籽中的残留量[J].南京医科大学学报(自然科学版),2004,24(4):425-426.
[5]庞帅,丁小霞,李培武,等.HPLC-MS/MS法测定花生中5种常用农药残留量[J].中国油料作物学报,2015,37(2):246-249.
[6]孙慧,侯志广,钱永盛,等.大豆中戊唑醇的气相色谱分析方法研究[J].安徽农业科学,2011,39(15):9029-9030.
[7]陈树兵,钟莺莺,贺小雨,等.高效液相色谱-电喷雾电离串联质谱法同时测定大豆中167种农药残留[J].分析测试学报,2014,33(5):499-505.
[8]朱臻怡,冯民,何健,等.固相萃取-气相色谱法同时测定花生中18种有机氯农药残留[J].化学分析计量,2010,19(1):19-22.
[9]贝峰,崔淑华,李杰,等.MSPD/GPC-GC-NCI/MS法测定花生及其制品中68种菊酯类农药残留方法的研究[J].分析测试学报,2012,31(s1):1-7.
[10]王明泰,牟峻,吴剑,等.GC-MS法测定粮谷及油料中55种有机磷农药残留量[J].分析试验室,2006,25(11):110-117.
[11]KOESUKWIWAT U,LEHOTAY S J,MASTOVSKA K,et al.Extension of the QuEChERS method for pesticide residues in cereals to flaxseeds,peanuts,and doughs[J].Journal of Agricultural&Food Chemistry,2010,58:5950-5958.
[12]宫兆晶,李培武,张文,等.基质固相分散-气相色谱法测定油菜籽中多种有机磷农药残留[J].中国油料作物学报,2007,29(3):333-338.
[13]胡敏,李二虎,吴兵兵,等.气相色谱法测定大豆中氟乐灵、甲草胺和乙草胺农药残留[J].现代农药,2006,5(6):27-28.
[14]LI Z,LI Y,LIU X,et al.Multiresidue analysis of 58 pesticides in bean products by disposable pipet extraction(DPX)cleanup and gas chromatography-mass spectrometry determination[J].Journal of Agricultural and Food Chemistry,2012,60(19):4788-4798.
[15]LI N,WANG Z,ZHANG L,et al.Liquid-phase extraction coupled with metal-organic frameworks-based dispersive solid phase extraction of herbicides in peanuts[J].Talanta,2014,128:345-353.