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用于定量检测禽蛋中青霉素G残留量的气相色谱-串联质谱法的建立与验证

Establishment and Validation of a GC-MS/MS Method for the Quantification of Penicillin G Residues in Poultry Eggs.

作者信息

Liu Chujun, Guo Yawen, Wang Bo, Chen Lan, Xie Kaizhou, Yang Chenggen

机构信息

College of Animal Science and Technology, Yangzhou University, Yangzhou 225009, China.

Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China.

出版信息

Foods. 2021 Nov 9;10(11):2735. doi: 10.3390/foods10112735.

Abstract

A simple and sensitive gas chromatography-tandem mass spectrometry (GC-MS/MS) method was established for the quantitative screening of penicillin G residues in chicken and duck eggs (whole egg, yolk and albumen). The analyte was separated on a TG-1MS capillary column (30.0 m × 0.25 mm i.d., 0.25 μm) with an external calibration method and electron impact (EI) ionization. Samples were pretreated using an accelerated solvent extraction (ASE) procedure followed by solid-phase extraction (SPE) on HLB cartridges (60 mg/3 mL). The derivative, which was safer and easier to store than penicillin G, was obtained by reacting trimethylsilyl diazomethane (TMSD) with penicillin G. The method was validated by the following parameters: linearity, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ). The matrix-matched calibration curves had good linearity (R2 ≥ 0.9994) within the concentration range of LOQ-200.0 µg/kg for penicillin G in the sample matrices. In the same concentration range, the accuracy, in terms of recovery, was 80.31-94.50%; the relative standard deviation (RSD), intra-day RSD and inter-day RSD ranged from 1.24 to 3.44%, 2.13 to 4.82% and 2.74 to 6.13%, respectively. The LODs and LOQs of penicillin G in the matrices were in the ranges of 1.70-3.20 and 6.10-8.50 μg/kg, respectively. The applicability of the GC-MS/MS method was demonstrated by the determination of poultry eggs obtained from local markets with no penicillin G residues.

摘要

建立了一种简单灵敏的气相色谱-串联质谱法(GC-MS/MS),用于定量筛查鸡鸭蛋(全蛋、蛋黄和蛋清)中的青霉素G残留量。分析物在TG-1MS毛细管柱(30.0 m×0.25 mm内径,0.25μm)上分离,采用外标法和电子轰击(EI)电离。样品采用加速溶剂萃取(ASE)程序进行预处理,然后在HLB小柱(60 mg/3 mL)上进行固相萃取(SPE)。通过三甲基硅基重氮甲烷(TMSD)与青霉素G反应得到比青霉素G更安全、更易于储存的衍生物。该方法通过以下参数进行验证:线性、准确度、精密度、检测限(LOD)和定量限(LOQ)。基质匹配校准曲线在样品基质中青霉素G的LOQ-200.0μg/kg浓度范围内具有良好的线性(R2≥0.9994)。在相同浓度范围内,回收率表示的准确度为80.31-94.50%;相对标准偏差(RSD)、日内RSD和日间RSD分别为1.24至3.44%、2.13至4.82%和2.74至6.13%。基质中青霉素G的LOD和LOQ分别在1.70-3.20和6.10-8.50μg/kg范围内。通过测定当地市场获得的无青霉素G残留的禽蛋,证明了GC-MS/MS方法的适用性。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/74f9/8621557/051faa436232/foods-10-02735-g001.jpg

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