牛、羊奶中莫昔克丁残留高效液相色谱荧光检测方法的建立  

Determination of Moxidectin Residue in Milk by High Performance Liquid Chromatography-fluorescence Detection Method

作　　者：沈昕 张玉洁[1] 李丹[1] 孙红洋 朱馨乐[1] 黄耀凌[1] SHEN Xin;ZHANG Yu-Jie;LI Dan;SUN Hong-Yang;ZHU Xin-le;HUANG Yao-ling(China Institute of Veterinary Drug Control,Beijing 100081,China)

机构地区：[1]中国兽医药品监察所,北京100081

出　　处：《中国兽药杂志》2021年第8期22-26,共5页Chinese Journal of Veterinary Drug

摘　　要：建立了适用于牛、羊奶样品中莫昔克丁残留的高效液相色谱荧光检测方法。以乙腈为提取液,C18固相萃取柱净化,并用N-甲基咪唑-乙腈(1+1,V/V)和三氟乙酸酐-乙腈(1+2,V/V)进行衍生化。乙腈+水(90+10,V/V)为流动相,荧光法定量。经测定,该方法对牛、羊奶中莫昔克丁的检测限为2μg/kg,定量限为5μg/kg。空白牛、羊奶中标准品莫昔克丁添加量分别为5、20、40和80μg/kg时,牛奶中莫昔克丁平均回收率范围为75.5%~110%,其批内变异系数小于7.38%,批间变异系数小于7.87%;羊奶中莫昔克丁平均回收率范围为77.5%~95.6%,其批内变异系数小于5.06%,批间变异系数小于5.92%。该方法准确性强、灵敏度高,适用于牛、羊奶中莫昔克丁的快速检测。A method for determination of moxidectin residue in bovine and ovine milk by high performance liquid chromatography-fluorescence detection(HPLC-FLD)was established.The analyte were extracted with acetonitrile and cleaning with C18 solid phase extraction column,using N-methylimidazole+acetonitrile(1+1,V/V)and trifiuoroacetic anhydride+acetonitrile(1+2,V/V)as the derivatization reagents.The mobile phase was acetonitrile and water(90+10,V/V)with equivalent elution,quantified by HPLC-FLD.The validation results showed that the limit of detection(LOD)of the method was 2μg/kg,and the limit of quantification(LOQ)was 5μg/kg in milk.Meanwhile,at the concentrations of 5,20,40 and 80μg/kg in moxidectin spiked blank milk,the average recoveries of this method were 75.5%~110%,with the intra-day coefficient variation(CVd)were less than 7.38%,inter-day coefficient variation(CVr)were less than 7.87%;the recoveries ranged from 77.5%to 95.6%,with the CVd were less than 5.06%,CVr were less than 5.92%.All of the above results show that this HPLC method has well practicability and accuracy,whitch could be applied in the rapid determination of moxidectin in milk.

关 键 词：牛、羊奶 莫昔克丁 残留 高效液相色谱荧光法 

分 类 号：S859.84[农业科学—临床兽医学]