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

建立和验证GC-MS/MS法定量测定禽蛋中青霉素G残留的方法

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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.

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