高效液相色谱法测定动物可食性组织中莫昔克丁残留量

Determination of Moxidectin Residue in Edible Tissues of Bovine and Ovine by High Performance Liquid Chromatography Method

关键词:  莫昔克丁  残留  高效液相色谱

Key words:  moxidectin  residue  high performance liquid chromatography

摘要:

建立了适用于检测畜肉及内脏中莫昔克丁残留的高效液相色谱法。样品经乙腈提取,加水混合后,C₁₈固相萃取柱净化,氮气吹干。将N-甲基咪唑-乙腈(1+1,v/v)和三氟乙酸酐-乙腈(1+2,v/v)作为衍生化试剂,65 ℃避光反应15 min进行衍生化。以乙腈+水(90+10,v /v)作为流动相,等度洗脱,荧光法测定。结果显示：莫昔克丁在线性范围内呈良好线性关系,相关系数(R^₂)大于0.999,检测限和定量限分别为2 μg/kg和5 μg/kg。该方法在以上各组织中的回收率范围为60.5 % ～ 110 %,其批间、批内变异系数范围为0.62 % ～ 15.8 %。该方法准确性强、灵敏度高,可满足实验室实际工作需求。

Abstract:

To develop a method capable of the simultaneously determining moxidectin in edible tissues of bovine and ovine, we established a high performance liquid chromatography method. After the sample were extracted with acetonitrile, the whole of supernatant was purified with C18 column, then evaporation. Using N－methylimidazole + acetonitrile(1+1，V/V) and trifiuoroacetic anhydride + acetonitrile(1+2，V/V) as the derivatization reagents, reactions at 65 ℃ in dark for 15 mins．The mobile phase was acetonitrile and water(90+10，V/V) with equivalent elution，quantified by HPLC-FLD. The results showed that a good linearity of the calibration curve of moxidectin was obtained in linear range, and the correlation coefficients (R2) were more than 0.999；The validation results showed that the limit of detection (LOD) and limit of quantification (LOQ) were 2 μg/kg and 5 μg/kg. Meanwhile，the average recoveries of this method were 60.5%～110% in various matrices, and the relative standard deviations for precision were 0.62% ~ 15.8%. All of the above results show that this HPLC method has well practicability and accuracy，which can meet the demand of determination of moxidectin in various laboratories．