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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
沈昕,张玉洁,李丹,孙红洋,朱馨乐,黄耀凌
0
(中国兽医药品监察所)
摘要:
建立适用于牛、羊奶样品中莫昔克丁残留的高效液相色谱荧光检测方法。本方法以乙腈为提取液,用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。以乙腈+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2 μg/kg,定量限为5 μg/kg。空白牛、羊奶中标准品莫昔克丁添加量分别为5、20、40和80 μg/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。
关键词:  牛、羊奶  莫昔克丁  残留  高效液相色谱荧光法
DOI:
投稿时间:2020-12-25修订日期:2021-05-28
基金项目:
Determination of Moxidectin residue in milk by high performance liquid chromatography-fluorescence detection method
(China Institute of Veterinary Drug Control)
Abstract:
To establish a method for determination of moxidectin residue in milk by high performance liquid chromatography-fluorescence detection (HPLC-FLD). The method by extracting the analyte 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 2 μg/kg, and the limit of quantification (LOQ) was 5 μg/kg in milk. Meanwhile, at the Moxidectin from spiked blank milk at the concentrations of 5、20、40 and 80 μg/kg , the average recoveries of this method for milk 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%~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,which can meet the demand of determination of cefquinome in various laboratories.The method was accuracy and sensitive, whitch could be applied in the rapid determination of moxidectin in milk.
Key words:  milk  Moxidectin  residue  HPLC-FLD

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