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分散液液微萃取后,采用毛细管区带电泳串联质谱法测定肉类样品中的苯并咪唑类化合物。

Determination of benzimidazoles in meat samples by capillary zone electrophoresis tandem mass spectrometry following dispersive liquid-liquid microextraction.

作者信息

Tejada-Casado Carmen, Moreno-González David, Lara Francisco J, García-Campaña Ana M, Del Olmo-Iruela Monsalud

机构信息

Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Av. Fuentenueva s/n, E-18071 Granada, Spain.

Department of Analytical Chemistry, Faculty of Sciences, University of Granada, Av. Fuentenueva s/n, E-18071 Granada, Spain.

出版信息

J Chromatogr A. 2017 Mar 24;1490:212-219. doi: 10.1016/j.chroma.2017.02.023. Epub 2017 Feb 14.

DOI:10.1016/j.chroma.2017.02.023
PMID:28222859
Abstract

A novel method based on capillary zone electrophoresis-tandem mass spectrometry has been proposed and validated for the identification and simultaneous quantification of twelve benzimidazoles in meat samples. Electrophoretic separation was carried out using 500mM formic acid (pH 2.2) as background electrolyte and applying a voltage of 25kV at 25°C. In order to improve the sensitivity, stacking mode injection was applied, using as injection solvent a mixture of 30:70 acetonitrile/water at 50mbar for 75s. Sensitivity enhancement factors from 74 to 317 were obtained under these conditions. Detection using an ion trap as analyzer, operating in multiple reactions monitoring mode was employed. The main MS/MS parameters as well as the composition of the sheath liquid and other electrospray variables were optimized in order to obtain the highest sensitivity and precision in conjunction with an unequivocal identification. The method was applied to poultry and pork muscle samples. The deproteinization of samples and extraction of benzimidazoles was carried out with acetonitrile. MgSO and NaCl were added as salting-out agents. Subsequently, dispersive liquid-liquid microextraction was applied as clean up procedure. The organic layer (acetonitrile, used as dispersant) containing the benzimidazoles was mixed with the extractant (chloroform) and both were injected in water, producing a cloudy solution. Recoveries for fortified samples were higher than 70%, with relative standard deviations lower than 16% were obtained in all cases. The limits of detection were below 3μgkg, demonstrating the applicability of this fast, simple, and environmentally friendly method.

摘要

一种基于毛细管区带电泳-串联质谱的新方法已被提出并验证,用于肉类样品中十二种苯并咪唑的鉴定和同时定量。电泳分离使用500mM甲酸(pH 2.2)作为背景电解质,在25°C下施加25kV电压进行。为了提高灵敏度,采用堆积模式进样,进样溶剂为30:70乙腈/水的混合物,在50mbar下进样75s。在这些条件下获得了74至317的灵敏度增强因子。使用离子阱作为分析仪,采用多反应监测模式进行检测。优化了主要的MS/MS参数以及鞘液组成和其他电喷雾变量,以便在明确鉴定的同时获得最高的灵敏度和精密度。该方法应用于家禽和猪肉肌肉样品。样品的脱蛋白和苯并咪唑的提取用乙腈进行。加入硫酸镁和氯化钠作为盐析剂。随后,采用分散液液微萃取作为净化程序。含有苯并咪唑的有机层(用作分散剂的乙腈)与萃取剂(氯仿)混合,两者都注入水中,产生浑浊溶液。加标样品的回收率高于70%,所有情况下相对标准偏差均低于16%。检测限低于3μg/kg,证明了这种快速、简单且环保方法的适用性。

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