摘要
采用QuEChERS及固相萃取样品前处理方法,结合液相色谱-三重四极杆串联质谱技术(LC-MS/MS),以负离子扫描和多反应监测模式(MRM),建立了菠菜、土壤及水体中螺虫乙酯及4种代谢物(B-enol、B-keto、B-mono和B-glu)残留的检测方法。通过对质谱检测条件的优化表明,以乙腈-0.5%甲酸水溶液作为流动相,采用梯度洗脱时,色谱分离度及灵敏度最好。通过对样品前处理条件的考察,发现选用0.1%甲酸-乙腈溶液作为提取溶剂,经50 mg的m(PSA):m(GCB)=1:1净化处理后,在0.05、0.5和1 mg/kg添加水平下,螺虫乙酯及4种代谢物在菠菜中的回收率为81%~103%,相对标准偏差(RSD)为1.7%~7.9%;在土壤样品中的回收率为82%~98%,RSD为1.9%~7.6%。采用NH2柱作为固相萃取柱,用10 m L二氯甲烷洗脱,在0.005、0.05和0.5 mg/L添加水平下,螺虫乙酯及4种代谢物在水体中的回收率为82%~95%,RSD为1.5%~6.2%。在0.002~1 mg/L范围内,螺虫乙酯及4种代谢物的质量浓度与对应的峰面积间呈现良好的线性关系,r在0.996 7~0.999 7之间。检出限(S/N=3)分别为螺虫乙酯(0.000 2~0.000 3 mg/kg),B-enol(0.000 1~0.000 3 mg/kg),B-keto(0.000 4~0.000 6 mg/kg),B-mono(0.000 4~0.000 7 mg/kg),B-glu(0.000 2~0.000 6 mg/kg);定量限(S/N=10)分别为螺虫乙酯(0.000 6~0.001 mg/kg),B-enol(0.000 3~0.001 mg/kg),B-keto(0.001 2~0.001 6 mg/kg),B-mono(0.001 2~0.001 9 mg/kg),B-glu(0.000 6~0.001 3 mg/kg)。方法分析结果符合农药残留检测要求,适用于菠菜、土壤及水体中螺虫乙酯及4种代谢物残留的同时检测。
A rapid and sensitive method based on QuEChERS and solid phase extraction using liquid chromatography-tandem mass spectrometry（LC-MS/MS） in negative ion scanning and multiple reaction monitoring（MRM） mode was developed for the residue detection of spirotetramat and its four metabolites（B-enol, B-keto, B-mono and B-glu） in Spinacia oleracea L., soil and water. When using aqueous phase of acetonitrile-0.5% formic acid as the mobile phase, gradient elution resulted in the best chromatographic resolution and sensitivity. When 0.1% formic acid-acetonitrile solution was used as the extraction solvent and the samples was purified by 50 mg m（PSA） ： m（GCB） = 1 ： 1, at the fortification levels of 0.05, 0.5 and 1mg/kg, the recoveries of spirotetramat and its four metabolites in spinach and soil were 81%-103% and 82%-98%, the RSD were 1.7%-7.9% and 1.9%-7.6%, respectively. The recoveries of spirotetramat and its four metabolites in water was 82%-95%, the RSD was 1.5%-6.2%, at the fortification levels of 0.005, 0.05 and 0.5 mg/L when the NH2 column was used as the solid phase extraction column and 10 m L of dichloromethane was used as the elution solvent. At concentrations ranging from 0.002-1 mg/L, there were good linear relationships between the mass concentration of spirotetramat and its four metabolites and the corresponding peak area, the correlation coefficients（r） were in the range 0.996 7-0.999 7. The limits of detection（S/N = 3） for all analytes were0.000 2-0.000 3 mg/kg（spirotetramat）, 0.000 1-0.000 3 mg/kg（B-enol）, 0.000 4-0.000 6 mg/kg（Bketo）, 0.000 4-0.000 7 mg/kg（B-mono）, 0.000 2-0.000 6 mg/kg（B-glu）, respectively. The limits of quantification（S/N = 10） for all analytes were 0.000 6-0.001 mg/kg（spirotetramat）, 0.000 3-0.001 mg/kg（B-enol）, 0.001 2-0.001 6 mg/kg（B-keto）, 0.001 2-0.001 9 mg/kg（B-mono）, 0.000 6-0.001 3 mg/kg（B-glu）, respectively. The method analysis results met the requirements for pesticide residue analysis. And this method
出处
《农药学学报》
CAS
CSCD
北大核心
2017年第4期482-490,共9页
Chinese Journal of Pesticide Science
基金
江苏省重点研发计划项目(现代农业)(BE2015354)
扬州市科技计划项目(YZ2015029)
扬州市科技计划(产学研合作专项)(YZ2016252)
关键词
液相色谱-串联质谱
菠菜
螺虫乙酯
代谢物
QUECHERS
固相萃取
残留
liquid chromatography-tandem mass spectrometry（LC-MS/MS）
Spinacia oleracea L
spirotetramat
metabolites
QuEChERS
solid phase extraction
residue
