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采用简单溶剂提取-液相色谱-电喷雾串联质谱法同时测定鸡蛋中的聚醚离子载体、大环内酯类和林可酰胺类抗生素

Simultaneous determination of polyether ionophores, macrolides and lincosamides in hen eggs by liquid chromatography-electrospray ionization tandem mass spectrometry using a simple solvent extraction.

机构信息

National Institute for Quality Control in Health/Oswaldo Cruz Foundation (INCQS/FIOCRUZ), Av. Brasil 4365, Rio de Janeiro, RJ, Brazil.

出版信息

Anal Chim Acta. 2010 Dec 3;682(1-2):82-92. doi: 10.1016/j.aca.2010.09.047. Epub 2010 Oct 7.

Abstract

A liquid chromatography-electrospray ionization tandem mass spectrometric (LC-ESI-MS/MS) method was developed and validated for the determination of residues of 6 polyether ionophores (lasalocid, maduramicin, monensin, narasin, salinomycin, semduramicin), 3 macrolides (erythromycin, tylosin, clarithromycin) and 1 lincosamide (lincomycin) in eggs. Nigericin was used as qualitative internal standard. Samples were deproteinizated/extracted with acetonitrile without pH adjustments. Aliquots of the extracts were evaporated and reconstituted for injection in the instrument operated in positive multiple reaction monitoring (MRM) mode. The stability of the antibiotics and the intensity of the formed ions were considered in order to select a suitable solvent for the reconstitution of the obtained dry extracts. No clean-up steps were required and matrix effects were controlled by sample dilution, selection of appropriate chromatographic conditions and reduced injection volume. Good within-laboratory reproducibility was obtained, with relative standard deviations (RSD(R)) from 4.0 (semduramicin at 5 μgkg(-1)) to 18.6 (erythromycin at 25 μgkg(-1)) for the ionophores and macrolides. Lincomycin showed the least precise results, with a maximum RSD(R) of 20.2% at 75 μgkg(-1)). Satisfactory decision limits (CCα) and detection capabilities (CCβ) were also attained. Method limits of detection (LODs) from 0.04 (salinomycin) to 1.6 μgkg(-1) (lincomycin) were achieved. Method limits of quantification (LOQs) were from 0.14 to 5.3 μgkg(-1) for the same drugs, respectively. All the LOQs, except that obtained for maduramicin were remarkably below the lowest validation level. The proposed method is suitable for routine application in commercial egg samples.

摘要

建立并验证了一种用于测定鸡蛋中 6 种聚醚类离子载体(拉沙洛西、马杜霉素、莫能菌素、那拉菌素、盐霉素、萨利霉素)、3 种大环内酯类(红霉素、泰乐菌素、克拉霉素)和 1 种林可酰胺类(林可霉素)残留量的液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)检测方法。奈替米星被用作定性内标。样品经乙腈沉淀/提取,无需调节 pH 值。提取液的等分试样经蒸发后,用正相多重反应监测(MRM)模式进样重新溶解。为了选择合适的溶剂来重新溶解获得的干提取物,考虑了抗生素的稳定性和形成离子的强度。无需进行净化步骤,通过样品稀释、选择合适的色谱条件和减少进样体积来控制基质效应。获得了良好的实验室重现性,对于离子载体和大环内酯,相对标准偏差(RSD(R))从 4.0(萨利霉素在 5μgkg(-1))到 18.6(红霉素在 25μgkg(-1))。林可霉素的结果最不精确,在 75μgkg(-1)时,RSD(R)最大为 20.2%。还达到了令人满意的决策界限(CCα)和检测能力(CCβ)。检测限(LOD)从 0.04(盐霉素)到 1.6μgkg(-1)(林可霉素)不等,定量限(LOQ)从 0.14 到 5.3μgkg(-1)不等。除了马杜霉素的 LOQ 外,所有的 LOQ 均显著低于最低验证水平。该方法适用于商业鸡蛋样品的常规应用。

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