超高效液相色谱-串联质谱法测定鳗鱼中呋线威和溴氰菊酯残留  被引量:17

Simultaneous Determination of Residual Furathiocarb and Deltamethrin in Eel by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry

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作  者:李永夫[1] 高华鹏 张健玲[3] 应跃康 吴志云 容文钦 

机构地区:[1]浙江林学院环境科技学院,临安311300 [2]徐龙食品集团有限公司,宁波315300 [3]江门出入境检验检疫局,江门529000

出  处:《分析化学》2008年第6期755-759,共5页Chinese Journal of Analytical Chemistry

摘  要:建立了同时快速测定鳗鱼中呋线威和溴氰菊酯残留的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法。样品以乙腈为提取剂,经脱脂、浓缩和净化,用流动相溶解,经超高效液相色谱分离,以串联质谱在多反应监测(MRM)模式下测定,在3.2min内完成呋线威和溴氰菊酯的定量分析。结果表明:呋线威和溴氰菊酯的标准曲线在0~10μg/kg浓度范围内线性良好,相关系数(r)分别为0.9998和0.9995;在1、5和10μg/kg添加水平条件下,呋线威和溴氰菊酯的加标回收率分别为83.4%~91.7%和85.6%~95.7%,相对标准偏差(RSD)均小于8%(n=6);本方法对呋线威和溴氰菊酯的定量限分别为0.07μg/kg和0.45μg/kg(S/N≥10)。Abstract An ultra performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method has been developed for the simultaneous determination of residual furathiocarb and dehamethrin in eel. The sample, extracted by acetonitrile, was finally dissolved in the mobile phase after the procedure of being defatted, concentration, and purification. Chromatographic separation was achieved by UPLC and the detection was performed by tandem mass spectrometry under the mode of multiple reaction monitoring. The quantitative analysis of furathiocarb and dehamethrin was finished in 3. 2 min. Results showed that in the range of 0 - 10 μg/kg the standard curves for furathiocarb and dehamethrin were in good linearity, and the correlation coefficients(r) were 0. 9998 and 0. 9995, respectively. The recoveries for furathiocarb and dehamethrin at the addition of three levels(1, 5, 10 g/kg) were 83.4% - 91.7% and 85.6% - 95.7% , respectively, and the relative standard deviation (RSD) for the determination of both furathiocarb and dehamethrin were less than 8% (n = 6). The limits of quantity( S/N ≥10) by the present method for furathiocarb and deltamethrin were found to be 0.07 μg/kg and 0.45 μg/kg, respectively.

关 键 词:超高效液相色谱-串联质谱法 鳗鱼 呋线威 溴氰菊酯 残留 

分 类 号:TS254.7[轻工技术与工程—水产品加工及贮藏工程]

 

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