摘要
建立了动物组织样品中洁霉素、氯洁霉素、红霉素、螺旋霉素、交沙霉素、泰乐菌素、竹桃霉素等7种林可酰胺类及大环内酯类药物多残留的液/质联用确证方法。用乙腈萃取样品中7种林可酰胺类及大环内酯类抗生素,然后用正己烷脱脂,旋转蒸发仪浓缩,以Luna C18(2)色谱柱为分离柱,在正离子模式下以电喷雾电离串联质谱仪进行测定。方法的检出限为0.05—5.3μg/kg。在20、50、200μg/kg 3个浓度水平进行验证实验,方法的线性范围为20-200μg/kg;总体平均回收率为70.3%~102%;相对标准偏差为2.4%~16.6%。本方法简便、快速、准确,各项技术指标满足国内外法规的要求,可用于动物组织样品中林可酰胺类及大环内酯类抗生素残留的确证检测。
A confirmative method was developed with high performance liquid chromatography tandem electrospray mass spectrometry (LC/MS/MS) to detect 7 residues of lincosamides and macrolides in animal tissues, which include lincomycin, clindamycin, tylosin, spiramycin, josamycin, erythromycin and oleandomycin. In the method, the 7 residues were extracted with acetonitrile, cleaned with hexane, and concentrated by rotary evaporator. Then the reconstituted sample solution was analyzed by LC/MS/MS in positive ion mode, with Luna C18 (2) column as the separation column. The limits of detection of the method are between 0.05 μg/kg and 5.3 μg/kg. The method is validated at 20 μg/kg, 50 μg/kg and 200 μg/kg level. The validation results were as follows: the linear range was from 20 μg/kg to 200μg/kg; the overall recovery varies from 70.3% to 102%, and the relative standard deviation (RSD) was between 2.4% and 16.6%. The method is simple, rapid, and accurate, and its performance can meet the requirements of the domestic and international legislation. The method adapts to simultaneously confirm residues of lincosamides and macrolides in animal tissue.
出处
《分析化学》
SCIE
EI
CAS
CSCD
北大核心
2007年第9期1290-1294,共5页
Chinese Journal of Analytical Chemistry
基金
深圳出入境检验检疫局科研基金资助项目(No.SZK03-2003)
关键词
液相色谱串联质谱
动物组织
林可酰胺类
大环内酯类
High performance liquid chromagography tandem mass spectrometry, animal tissue, lincosamides, macrolides
作者简介
E-mail:yuezhenfeng@163.com