摘要
为建立鸡组织(肌肉、肝脏、肾脏)中脱氢乙酸(DHA)残留的高效液相色谱(HPLC)检测方法,将鸡组织样品经乙腈提取,正己烷液-液萃取,PAX小柱固相萃取净化后,用乙腈溶解残渣,过滤,HPLC分析。色谱条件为:甲醇-0.02%乙酸铵缓冲溶液(20/80,v/v)为流动相,290nm紫外检测。DHA标准工作液在0.2~5.0mg/L浓度范围内线性关系良好(R2≥0.9996),方法检测限为0.1mg/kg,定量限为0.2mg/kg。各组织中DHA添加浓度为0.5、1.0、5.0mg/kg时,各组织样品中DHA回收率为68.28%~93.49%,日内变异系数在3.38%~7.94%,日间变异系数在4.31%~7.80%。所建立的HPLC方法能够满足动物性组织中DHA的残留检测,可为DHA在动物性食品中的残留消除、最高残留限量及休药期研究提供技术支持。
A high performance liquid chromatography (HPLC)method was established to determine the residues of dehydroaeetic acid (DHA)in chicken tissues. The tissue samples (muscle,liver and kidney)were extracted with acetonitrile, liquid-liquid extraction by hexane, purified by PAX solid phase extraction column. A C18 column with ultraviolet absorption detection at 290 nm,using methanol-water which includes 0.02% ammonium acetate (20/80,v/v)as eluent was used in HPLC. A linear calibration curve with coefficient relation (R2≥0.9996) in the range of 0.2 to 5.0 mg/L of DHA concentration was made. When DHA was added to tissues at dose of 0.5,1.0 and 5.0 mg/kg,the average recover-ies in different tissues were ranged from 68.28% to 93.49%,with CV% ranged from 3.38% to 7.94% within-day and 4.31% to 7.80% between-day. The limit of detection and limit of quantitation of DHA were observed at 0.1 mg/kg and 0.2 mg/kg respeetively. The established method was suitable for the determination of DHA residues in animal foods,be also useful to the investigation of DHA depletion,the maximum residue limit and its withdraw time.
出处
《中国家禽》
北大核心
2012年第24期25-28,共4页
China Poultry
基金
中央高校基本科研业务费专项资金(JKQ2011011)
关键词
脱氢乙酸
药物残留
HPLC
鸡组织
dehydroacetic acid
high performance liquid chromatography
drug residue
chicken tissue
作者简介
通讯作者,E-mail:ymzhnet@sina.com