Liu Chujun, Guo Yawen, Wang Bo, Chen Lan, Xie Kaizhou, Yang Chenggen
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.
Foods. 2021 Nov 9;10(11):2735. doi: 10.3390/foods10112735.
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.
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。