摘要
本研究旨在开发一种高效、经济的方法,利用高效能液相层析仪(HPLC)配合光二极管侦测器(PDA),对饲料中乙烯雌酚含量进行分析。为了避免在低浓度情况下的误判,同时采用高效液相层析质谱仪(HPLC/MS)进行了再确认。在实验中,饲料样品以甲醇为萃取液,经过振荡、离心、浓缩上清液,残渣用70%甲醇溶解,通过Oasis■HLB卡匣去除干扰物质,最后用甲醇进行冲提,冲提液经高效液相层析仪检测。实验结果表明,对于饲料添加0.5、1、3、5 ppm的情况,回收率在80.8%到107.5%。仅采用光二极管侦测器检测时,最低检测限为0.03 ppm;而采用质谱侦测器检测时,最低检测限可达0.005 ppm。研究结果表明,所开发的高效液相层析仪饲料中乙烯雌酚检测方法具有便捷、经济、可行的特点,可作为饲料中乙烯雌酚检验的一种有效方法。
This study aims to develop an efficient and economical method to analyze the content of diethylstilbestrol in feed using high-performance liquid chromatography(HPLC)and photodiode detector(PDA).In order to avoid misjudgment at low concentrations,high-performance liquid chromatography mass spectrometry(HPLC/MS)was also used for re-confirmation.In the experiment,the feed samples were extracted with methanol.After shaking,centrifugation,and concentration of the supernatant,the residue was dissolved in 70% methanol,and interfering substances were removed through the Oasis■HLB cassette.Finally,it was rinsed with methanol,and detected with high performance liquid chromatography.Experimental results show that when 0.5 ppm,1 ppm,3 ppm,and 5 ppm are added to feed,the recovery rate is between 80.8% and 107.5%.When using only a photodiode detector,the minimum detection limit is 0.03 ppm;when using a mass spectrometer detector,the minimum detection limit can reach 0.005 ppm.The research results show that the developed high-performance liquid chromatography method for detecting diethylstilbestrol in feed is convenient,economical,and feasible,and can be used as an effective method for detecting diethylstilbestrol in feed.
作者
李东
单晓丽
周峰
LI Dong;SHAN Xiao-li;ZHOU Feng(Anqiu Inspection and Testing Center Co.,Ltd.)
出处
《中国标准化》
2024年第10期200-203,共4页
China Standardization
