Wang Bo, Wang Yajuan, Xie Xing, Diao Zhixiang, Xie Kaizhou, Zhang Genxi, Zhang Tao, Dai Guojun
College of Veterinary Medicine, Yangzhou University, Yangzhou 225009, China.
Joint International Research Laboratory of Agriculture & Agri-Product Safety, Yangzhou University, Yangzhou 225009, China.
Foods. 2020 May 18;9(5):651. doi: 10.3390/foods9050651.
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.
建立了一种基于加速溶剂萃取（ASE）结合气相色谱串联质谱（GC-MS/MS）的方法，用于定量分析禽蛋（全蛋、蛋清和蛋黄）样品中的壮观霉素和林可霉素。在本研究中，使用ASE350仪器和固相萃取（SPE）柱对样品进行萃取和净化，并通过实验优化了ASE方法的参数。选择了合适的SPE柱，并优化了衍生化反应条件。衍生化后，采用GC-MS/MS对禽蛋（全蛋、蛋清和蛋黄）样品进行分析。本研究使用空白禽蛋（全蛋、蛋清和蛋黄）样品评估该方法的特异性、灵敏度、线性、回收率和精密度。该方法的线性范围（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（相对标准偏差为1.0% - 3.4%）、检测限（2.3 - 4.3μg/kg）和定量限（5.6 - 9.5μg/kg）均符合欧盟参数验证要求。与传统液液萃取方法相比，该方法快速且试剂消耗少，一次可处理24个样品。最后，通过实际样品检测评估了该方法的可行性，成功检测出禽蛋中的壮观霉素和林可霉素残留。
