高效液相色谱-串联质谱法快速检测马铃薯与土壤中氟醚菌酰胺残留
投稿时间:2017-08-02      点此下载全文 HTML
引用本文:冯义志,李颖,金杰,潘金菊,唐剑峰,齐晓雪,梁林,张爱娟,刘伟,等.高效液相色谱-串联质谱法快速检测马铃薯与土壤中氟醚菌酰胺残留[J].农药学学报,2017,19(6):760-764.
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冯义志 山东省农药科学研究院 山东省化学农药重点实验室, 济南 250033  
李颖 山东省联合农药工业有限公司, 济南 250100  
金杰 山东省农药科学研究院 山东省化学农药重点实验室, 济南 250033  
潘金菊 山东省农药科学研究院 山东省化学农药重点实验室, 济南 250033  
唐剑峰 山东省联合农药工业有限公司, 济南 250100  
齐晓雪 山东省农药科学研究院 山东省化学农药重点实验室, 济南 250033  
梁林 山东省农药科学研究院 山东省化学农药重点实验室, 济南 250033  
张爱娟 山东省农药科学研究院 山东省化学农药重点实验室, 济南 250033  
刘伟 山东省农药科学研究院 山东省化学农药重点实验室, 济南 250033 liuwhx1988@163.com 
中文摘要:建立了采用QuEChERS为样品前处理方法的高效液相色谱-串联质谱(HPLC-MS/MS)快速检测马铃薯和土壤中氟醚菌酰胺残留的分析方法。样品经乙腈提取,PSA、C18吸附剂净化,电喷雾电离、正离子模式采集,多反应监测模式检测,基质匹配标准品外标法定量。结果表明:在0.002~1 mg/L范围内,氟醚菌酰胺在马铃薯等基质中的质量浓度与对应的峰面积间呈良好的线性关系,其相关系数均大于0.999 9。在 0.005~0.5 mg/kg添加水平下,氟醚菌酰胺在马铃薯、马铃薯植株和土壤中的日内平均回收率为81%~98%,日内相对标准偏差(RSD)为2.2%~13%(n = 5);日间平均回收率为75%~106%,日间RSD为0.6%~11%(n = 15)。氟醚菌酰胺在马铃薯等基质中的定量限(LOQ)(S/N=10)均为0.001mg/kg。该方法简便、快速、准确,可用于马铃薯中氟醚菌酰胺的残留检测。
中文关键词:高效液相色谱-串联质谱  马铃薯  土壤  杀菌剂  氟醚菌酰胺  残留
 
Determination of LH-2010A residues in potato and soil
Abstract:A rapid and sensitive analytical method for the determination of LH-2010A residues in potato and soil was established based on QuEChERS(Quick, Easy, Cheap, Effective, Rugged and Safe) and high performance liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). The samples were extracted with acetonitrile, and purified with primary secondary amine (PSA) and octadecylsilane (C18). The mass spectrometer was performed in multi-reaction monitoring mode, and electrospray ionization in positive mode was selected. The LH-2010A residues were quantified by the external standard method using the matched standard solution to compensate for matrix effect. The results indicated that the calibration curves of LH-2010A were linear in the range of 0.002-1 mg/L with correlation coefficients of more than 0.999 9. When the addition level ranged from 0.005 to 0.5mg/kg, the intra-day average recoveries of LH-2010A in potato, potato plant and soil were 81%-98%, and the relative standard deviation (RSD) ranged from 2.2% to 13% (n = 5). The inter-day average recoveries of LH-2010A were 75%-106%, and with RSD ranged from 0.6% to 11% (n = 15). The limit of quantitation (LOQ) were 0.001 mg/kg in different matrices. This method is simple, rapid and accurate, and can be adapted for the confirmation of LH-2010A residues in potato samples.
Key words:high performance liquid chromatography-tandem mass spectrometry  potato  soil  fungicide  LH-2010A  residues
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