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.
Keywords: ASE; GC-EI/MS/MS; lincomycin; poultry eggs; spectinomycin.