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牛奶中4种阿维菌素类药物的高效液相色谱快速测定
程林丽1, 安洪泽2, 沈建忠1, 曹斌斌1, 黄兴华1
0
(1.中国农业大学 动物医学院,北京 100193;2.中国兽医药品监察所,北京 100081)
摘要:
用乙腈提取牛奶中残留的4种阿维菌素类药物,加水和微量三乙胺稀释,C18固相萃取柱净化,氮气吹干并衍生化后用高效液相色谱-荧光检测法测定,外标法定量。结果表明:在2~5 000 μg/L质量浓度范围内,4种药物的浓度与峰面积均呈线性相关,相关系数≥0.99。对不含阿维菌素类药物残留的牛奶进行2~1 000 μg/kg药物添加回收实验,结果表明:各药物的回收率为70.2 %~110.4%,批内变异系数为3.9%~8.2%,批间变异系数5.1%~8.2%。按3倍信噪比计算,本方法对埃普利诺菌素、阿维菌素、多拉菌素和伊维菌素的检测限依次为0.5、0.5、0.4和0.2 μg/kg;按10倍信噪比计算,定量限依次为1.8、1.6、1.3和0.8 μg/kg。该方法简单、准确、灵敏,适用于牛奶中阿维菌素类药物的多残留检测。
关键词:  牛奶  阿维菌素类  残留  C18固相萃取  高效液相色谱法  荧光检测
DOI:10.11841/j.issn.1007-4333.2010.04.016
投稿时间:2009-11-09
基金项目:
Rapid HPLC for quantitation of 4 kinds of avermectin residues in milk
CHENG Lin-li1, AN Hong-ze2, SHEN Jian-zhong1, CAO Bin-bin1, HUANG Xing-hua1
(1.College of Veterinary Medicine,China Agricultural University,Beijing 100193,China;2.China Institute of Veterinary Drug Control,Beijing 100081,China)
Abstract:
Avermectins were simply extracted with acetonitrile from milk.The sample solution was diluted with water and mini triethylamine.Avermectins were selectively concentrated by one 500 mg C18 cartridge.The elution was evaporated to dryness and derivatized,and then was determined by HPLC with fluorescence detection.The results showed that the concentrations of the four drugs were linearly correlated with their peak areas and the coefficient ≥0.99.The average recoveries of 4 target drugs range from 70.2% to 110.4% when spiked 2-1 000 μg/kg.The intra-coefficients of variation were in the range of 3.9%-8.2% and the inter-coefficients of variation were in the range of 5.1%-8.2%.The limit of detection was 0.5,0.5,0.4 and 0.2 μg/kg for eprinomectin,avermectin,doramectin and ivermectin,respectively,when calculated with 3 S/N.And the quantitation limit was 1.8,1.6,1.3 and 0.8 μg/kg,respectively.The most significant aspect of the present study was the much simplified sample preparation procedure.Only one reverse SPE without additional cleanup method was used for preparing samples.It is a rapid,specific,and sensitive method for determination of avermectin residues in milk.
Key words:  milk  avermectins  residue  C18 solid phase extraction  HPLC  fluorescence detection