QuEChERS-液相色谱-串联质谱法测定牛蛙肉中酰胺醇类抗生素及其代谢物

采用QuEChERS技术提取氯霉素、甲砜霉素、氟苯尼考及其代谢物氟苯尼考胺,建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)同时测定牛蛙肉中酰胺醇类抗生素及其代谢物的检测方法。结果表明:在0.1~50.0 ng/mL范围内,酰胺醇类抗生素及其代谢物质量浓度与其质谱响应值呈良好的线性关系,相关系数均大于0.999 1;检出限为0.007 5~0.003 0 μg/kg,定量限为0.025~0.100 μg/kg;加标回收率为94.3%~97.9%,相对标准偏差为0.8%~3.7%。

Determination of Amphenicol Antibiotics and Metabolite Residues in Bullfrog Meat by QuEChERS-Liquid Chromatography-Tandem Mass Spectrometry

A quick, easy, cheap, effective, rugged and safe (QuEChER) extraction procedure followed by a liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay was established for the simultaneous determination of amphenicol antibiotics (chloramphenicol, thiabendazole and florfenicol) and the florfenicol metabolite florfenicol amine (FFA) in bullfrog meat. The results showed that there was a good linear relationship between the mass spectrometric response and concentrations of all analytes in the range from 0.1 to 50.0 ng/mL with correlation coefficients all greater than 0.999 1. The limits of detection and quantitation were in the range from 0.007 5 to 0.003 0 μg/kg and from 0.025 to 0.100 μg/kg, respectively. The recoveries from spiked samples were in the range from 94.3% to 97.9%, with relative standard deviation of 0.8% to 3.7%.