液相色谱-串联质谱法同时测定菠菜、土壤及水体中螺虫乙酯及4种代谢物残留
投稿时间:2017-05-17      点此下载全文 HTML
引用本文:孟志远,任莉,宋玥颐,徐志英,陈小军,等.液相色谱-串联质谱法同时测定菠菜、土壤及水体中螺虫乙酯及4种代谢物残留[J].农药学学报,2017,19(4):482-490.
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孟志远 扬州大学 园艺与植物保护学院/农业与农产品安全国际合作联合实验室 (扬州大学), 江苏 扬州 225009  
任莉 扬州大学 园艺与植物保护学院/农业与农产品安全国际合作联合实验室 (扬州大学), 江苏 扬州 225009  
宋玥颐 扬州大学 园艺与植物保护学院/农业与农产品安全国际合作联合实验室 (扬州大学), 江苏 扬州 225009  
徐志英 扬州市职业大学, 江苏 扬州 225009  
陈小军 扬州大学 园艺与植物保护学院/农业与农产品安全国际合作联合实验室 (扬州大学), 江苏 扬州 225009 cxj@yzu.edu.cn 
基金项目: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)
中文摘要: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 mL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。
中文关键词:液相色谱-串联质谱  菠菜  螺虫乙酯  代谢物  QuEChERS  固相萃取  残留
 
Simultaneous determination of spirotetramat and its four metabolites in Spinacia oleracea L., soil and water using liquid chromatography-tandem mass spectrometry
Abstract: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 mL 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 were 0.000 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 (B-keto), 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 is applicable to simultaneous detection of spirotetramat and its four metabolites in spinach, soil and water.
Key words:liquid chromatography-tandem mass spectrometry (LC-MS/MS)  Spinacia oleracea L.  spirotetramat  metabolites  QuEChERS  solid phase extraction  residue
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