超高效液相色谱-串联质谱法检测鸡肉中大环内酯类药物残留量

Determination of Macrolides Residue in Chicken by Ultra-high Performance Liquid Chromatography-tandem Mass Spectrometry

建立鸡肉中3种大环内酯类药物的高效液相色谱-串联四级杆质谱(UPLC-MS/MS)残留分析方法。样本在乙腈水溶液提取下经PRIME HLB固相萃取柱净化,氮吹浓缩后定容过膜上机检测。在1.00~50.0μg/L线性范围内,竹桃霉素、克林霉素、交沙霉素的标准曲线相关系数分别为r=0.99994、r=0.99982、r=0.99962,方法检出限分别为0.59μg/kg、0.72μg/kg、0.48μg/kg。加标回收试验中竹桃霉素、克林霉素、交沙霉素加标浓度分别为3.00μg/kg、6.00μg/kg、30.0μg/kg,回收率范围分别为83.7%~102.8%,87.0%~110.0%,76.2%~103.0%。本方法适用于可食动物肌肉竹桃霉素、克林霉素、交沙霉素残留的检测。

A method for the residue analysis of 3 macrolides in chicken was established by ultra-high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. The samples were purified by PRIME HLB solid phase extraction column under the extraction of acetonitrile water. After drying and concentrating, the samples were reused and were tested over the membrane. In the linear range of 1.00 μg/L-50.0 μg/L, the correlation coefficient of the standard curve of Oleandomycin, clindamycin and josamycin was r=0.99994, r=0.99982 and r=0.99962, the detection limits were 0.59 μg/kg, 0.72 μg/kg and 0.48 μg/kg respectively. The recovery rate of Oleandomycin, clindamycin and josamycin respectively was 83.7 %-102.8 %, 87.0 %-110.0 %, 76.2 %-103.0 % in the adding standard recovery test when the Standard concentration respectively were 3 μg/kg, 6 μg/kg and 30 μg/kg. This method is suitable for the detection of edible animal muscle oleandomycin, clindamycin, josamycin residues.