Wu Xinyi, Shen Xixi, Cao Xiangyue, Nie Rongrong, Zhang Haonan, Tang Changbo, Wang Wei
Key Laboratory of Meat Processing and Quality Control, MOE, Key Laboratory of Meat Processing, MARA, Jiangsu Collaborative Innovation Center of Meat Production and Processing, Quality and Safety Control, College of Food Science and Technology, Nanjing Agricultural University, Nanjing 210095, China.
Int J Anal Chem. 2021 Nov 3;2021:3613670. doi: 10.1155/2021/3613670. eCollection 2021.
Amphenicols are widely used to prevent and treat animal diseases. However, amphenicol residues accumulate in livestock and poultry and harm consumers. We hypothesized that one can combine solid-phase extraction (SPE) with ultrahigh-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) to simultaneously determine amphenicols and metabolites in pork, beef, lamb, chicken, and their products and meet government regulations for maximum residue limits. We extracted crude samples with ethyl acetate and ammonia water (98:2, v/v), purified the samples with a CNW Si SPE column, defatted the samples with acetonitrile-saturated -hexane, and then determined the resulting analytes by UHPLC-MS/MS. The limit of detection of the analytes in livestock and poultry meat was 0.03-1.50 g/kg, and the limit of quantification was 0.05-5.00 g/kg. Measured chloramphenicol, thiamphenicol, and florfenicol concentrations were linear over the range 0.50-50 g/kg; and the florfenicol amine concentration was linear over the range 5.00-200 g/kg (all with correlation coefficients >0.9990). The recovery of the spiked samples was between 72% and 120%. The intraday relative standard deviation (RSD) ranged from 1% to 9%, and the interday RSD ranged from 1% to 12%. Based on the above results, the current method is sensitive, accurate, and reproducible with the detection limits being well below the maximum residue limits as per Chinese standard GB 31650-2019, and thus, our research hypothesis could be confirmed.
氯霉素类药物被广泛用于预防和治疗动物疾病。然而，氯霉素残留会在畜禽体内蓄积并危害消费者。我们推测，可以将固相萃取（SPE）与超高效液相色谱 - 串联质谱法（UHPLC - MS/MS）相结合，同时测定猪肉、牛肉、羊肉、鸡肉及其制品中的氯霉素类药物和代谢物，并符合政府规定的最大残留限量标准。我们用乙酸乙酯和氨水（98:2，v/v）提取粗样品，用CNW Si SPE柱净化样品，用乙腈饱和的正己烷脱脂样品，然后通过UHPLC - MS/MS测定所得分析物。畜禽肉中分析物的检测限为0.03 - 1.50 g/kg，定量限为0.05 - 5.00 g/kg。测得的氯霉素、甲砜霉素和氟苯尼考浓度在0.50 - 50 g/kg范围内呈线性；氟苯尼考胺浓度在5.00 - 200 g/kg范围内呈线性（所有相关系数均>0.9990）。加标样品的回收率在72%至120%之间。日内相对标准偏差（RSD）范围为1%至9%，日间RSD范围为1%至12%。基于上述结果，当前方法灵敏、准确且可重复，检测限远低于中国标准GB 31650 - 2019规定的最大残留限量，因此，我们的研究假设得到了证实。
