鸡蛋中洛克沙胂的检测方法及动态代谢规律的研究

Study on High Performance Liquid Chromatography Detection Method and Dynamic Metabolism of Roxarsone in Egg

建立了检测鸡蛋中洛克沙胂含量的高效液相色谱法(HPLC),并对鸡蛋中的洛克沙胂的动态残留进行了研究。鸡蛋经冷冻干燥后用甲醇+冰乙酸(9+1)提取剂提取,Diamond C18色谱柱,流动相为冰乙酸+三乙胺+甲醇,流速0.8ml/min,柱温30℃,进样量10μl,检测波长264nm。该方法的线性范围为0.50～10.0μg/ml,相关系数R2=0.9959,在三个添加浓度水平上的平均回收率分别为85.81%、85.61%和87.46%,检出限为0.1μg/ml,三次测定的相对标准偏差<1%(分别为0.35%、0.59%、0.95%)。初步得到了洛克沙胂在鸡蛋中的动态残留规律:鸡蛋中的洛克沙胂的残留量随着饲料中的洛克沙胂的添加量的增加而增加,最大值出现的时间也有所提前;停药后鸡蛋中的洛克沙胂的残留量显著减少,随着添加量的减少未检出的时间相应提前。

A high performance liquid chromatography （HPLC）method was developed for the determination of roxarsone in eggs, and the dynamic metabofism of roxarsone in egg was investigated. Egg powder made from egg liquid via freeze-drying was extracted with CH3OH ＋ CH3COOH （9：1）. The chromatographic separation was performed on a Diamond C18 column, using 500 ml H2O solution of 10 ml CH3COOH and 1.3 ml （C2H5）3N plus mixture of CH3OH and H2O （85%＋15%） as mobile phase at the rate of 0. 8 ml/min, under the condition of column temperature 30℃, injection quality 10 μl and ultraviolet detection wavelength 264 nm. Results showed that the linear range of this method is 0.50 μg/ml to 10.0 μg/ml with the correlation coefficient of 0.9959. The average recoveries of three different addition levels are 85.81%, 5.61% and 87.46%, respectively, the limit of detection is 0.1 μg/ml, and the RSDs of three detections are not more than 1% （0.35%, 0.59% and 0.95% respectively）.The dynamic metabolism rules of roxarsone in egg are： （1） the residue of roxarsone increases with the addition in the feed of hen rising and the appearance time of maximum is ahead. After drug withdrawal, the residue of roxarsone in egg reduces prominently and the time of no detection is advanced along with the decreasing of the addition quality in the feed of hen.