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Quantitative Analysis of Spectinomycin and Lincomycin in Poultry Eggs by Accelerated Solvent Extraction Coupled with Gas Chromatography Tandem Mass Spectrometry

机译:加速溶剂萃取-气相色谱串联质谱法定量分析禽蛋中大观霉素和林可霉素

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摘要

A method based on accelerated solvent extraction (ASE) coupled with gas chromatography tandem mass spectrometry (GC-MS/MS) was developed for the quantitative analysis of spectinomycin and lincomycin in poultry egg (whole egg, albumen and yolk) samples. In this work, the samples were extracted and purified using an ASE350 instrument and solid-phase extraction (SPE) cartridges, and the parameters of the ASE method were experimentally optimized. The appropriate SPE cartridges were selected, and the conditions for the derivatization reaction were optimized. After derivatization, the poultry egg (whole egg, albumen and yolk) samples were analyzed by GC-MS/MS. This study used blank poultry egg (whole egg, albumen and yolk) samples to evaluate the specificity, sensitivity, linearity, recovery and precision of the method. The linearity (5.6–2000 μg/kg for spectinomycin and 5.9–200 μg/kg for lincomycin), correlation coefficient (≥0.9991), recovery (80.0%–95.7%), precision (relative standard deviations, 1.0%–3.4%), limit of detection (2.3–4.3 μg/kg) and limit of quantification (5.6–9.5 μg/kg) of the method met the requirements for EU parameter verification. Compared with traditional liquid–liquid extraction methods, the proposed method is fast and consumes less reagents, and 24 samples can be processed at a time. Finally, the feasibility of the method was evaluated by testing real samples, and spectinomycin and lincomycin residues in poultry eggs were successfully detected.
机译:建立了一种基于加速溶剂萃取(ASE)和气相色谱串联质谱(GC-MS / MS)的方法,用于定量分析禽蛋(全蛋,蛋清和蛋黄)中的壮观霉素和林可霉素。在这项工作中,使用ASE350仪器和固相萃取(SPE)小柱对样品进行了提取和纯化,并对ASE方法的参数进行了实验优化。选择合适的SPE柱,并优化衍生化反应的条件。衍生后,通过GC-MS / MS分析禽蛋(全蛋,蛋清和蛋黄)样品。这项研究使用空白禽蛋(全蛋,蛋清和蛋黄)样品评估了该方法的特异性,敏感性,线性,回收率和精密度。线性度(壮观霉素为5.6–2000μg/ kg,林可霉素为5.9–200μg/ kg),相关系数(≥0.9991),回收率(80.0%–95.7%),精密度(相对标准偏差,1.0%–3.4%) ,方法的检出限(2.3–4.3μg/ kg)和定量限(5.6–9.5μg/ kg)符合EU参数验证的要求。与传统的液-液萃取方法相比,该方法快速且消耗的试剂更少,一次可处理24个样品。最后,通过测试实际样品评估了该方法的可行性,并成功检测了禽蛋中的壮观霉素和林可霉素残留。

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