采用基质固相分散技术( QuEChERS)为样品前处理方法,建立了高效液相色谱-串联质谱( HPLC-MS/MS)快速检测小麦植株、小麦粒和土壤中萎锈灵残留量的分析方法.样品经乙腈提取及盐析处理后,用N-丙基乙二胺(PSA)和石墨化碳黑(GCB)固相萃取填料净化,HPLC-MS/MS、多反应监测模式(MRM)下测定.基质标准曲线外标法进行定量分析.结果显示,在0.005—0.5 mg·L-1浓度范围内,不同基质中萎锈灵均有较好的线性关系(R2>0.998),在0.02、0.2、1 mg·kg-1添加水平下,萎锈灵在不同基质中的平均回收率介于77.5%—109.7%,相对标准偏差(RSD)介于1.7%—9.9%,检出限(LOD)为0.5 μg·L-1,方法的最低检测浓度( LOQ)均为0.02 mg·kg-1 .该方法前处理简单、快速,分析时间短,灵敏度、准确度和精密度均符合农药残留检测要求,适用于小麦样品中萎锈灵残留量的检测.
A rapid and sensitive analytical method for the determination of carboxin residues in wheat plant, grain and soil samples was developed and validated based on QuEChERS ( Quick, Easy, Cheap, Effective, Rugged, and Safe) and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The sample was extracted with acetonitrile. After addition of sodium chloride and centrifugation, the supernant was cleaned-up by N-propylethyl-diamine ( PSA)and graphitizing of carbon black ( GCB) , then determined by HPLC-MS/MS under multiple reaction monitoring mode ( MRM ) . Sample matrix-matched calibration was used to determine the residue contents by external standard. Over the concentration range of 0. 005—0. 5 mg·L-1 carboxin in different matrix, the correlation coefficients (R2) of the calibration curves were all above 0.998. The recovery of carboxin in different matrix at three spiked concentration levels of 0. 02, 0. 2 and 1 mg·kg-1 ranged from 77.5%to 109.7%, the relative standard deviation ( RSD) between 1.7%and 9.9% (n=5) and the limit of detection (LOD) was 0.5μg·L-1. Moreover, the limit of quantitation ( LOQ) in wheat plant, grain and soil were all 0. 02 mg·kg-1 . The method is simple, rapid and characterized with acceptable sensitivity and accuracy to meet the requirements of the pesticide residue analysis.The method is applicable to confirm the residues of carboxin in wheat samples.
参考文献
| [1] | 季汝泉.反相高效液相色谱法测定萎锈灵[J].安徽化工,2004(03):59-60. |
| [2] | 张浩;王岩;逯忠斌;徐威.卫福（carboxin+thiram）在水稻苗及土壤上的残留动态[J].吉林农业大学学报,2001(4):64-68. |
| [3] | 张志刚;郑向华;施冰;叶鹏;林立毅;陈鹭平;邹伟;庄宛;王根芳;方元炜;周昱.进口巴西"毒大豆"中种衣剂农药残留分析方法研究[J].检验检疫科学,2004(z1):6-10. |
| [4] | 徐娟;陈捷;叶弘毅;王岚;孙灵慧;赖子峰.QuEChERS提取与高效液相色谱-电喷雾电离串联质谱联用法检测茶叶中的19种农药残留[J].分析测试学报,2011(9):990-995. |
| [5] | 王玉健;黄惠玲;徐志伟;梁振纲;董存柱.高效液相色谱-串联质谱法测定茶叶中唑螨酯、三唑酮、鱼藤酮、除虫脲及萎锈灵残留量[J].理化检验-化学分册,2014(12):1526-1529. |
| [6] | Anastassiades M;Lehotay SJ;Stajnbaher D;Schenck FJ.Fast and easy multiresidue method employing acetonitrile extraction/partitioning and "dispersive solid-phase extraction" for the determination of pesticide residues in produce[J].Journal of AOAC International,20032(2):412-431. |
| [7] | 王旭;刘新刚;董丰收;安晶晶;郑永权.噻苯隆在甜瓜和土壤中的残留及消解动态[J].环境化学,2010(2):277-280. |
| [8] | 路彩红;刘新刚;董丰收;徐军;王旭;郑永权.烯啶虫胺在棉花和土壤中的残留及消解动态[J].环境化学,2010(4):614-618. |
| [9] | 曹文卿;林黎明;吴振兴;鲍蕾;梁成珠;杨桂朋.QuEChERS/液相色谱-串联质谱法测定红鳍东方鲀肉中河鲀毒素[J].分析测试学报,2014(5):588-593. |
| [10] | 段婷婷;张盈;魏进;朱峰.超高效液相色谱-串联质谱快速检测精米、玉米与土豆样品中噻呋酰胺残留[J].分析测试学报,2014(5):598-601. |
| [11] | 梁林;潘金菊;刘伟.超高效液相色谱-串联质谱法同时测定玉米及土壤中烟嘧磺隆和2甲4氯残留[J].农药学学报,2012(6):659-663. |
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