高效液相色谱法测定饲料中艾司唑仑的含量

Determination of Estazolam in feeds by High Performance Liquid Chromatography

关键词:  艾司唑仑,饲料,高效液相色谱

Key words:  Estazolam  feeds  high performance liquid chromatography(HPLC)

摘要:

本研究建立了高效液相色谱法测定预混合饲料、配合饲料和浓缩饲料中艾司唑仑含量的检测方法。试样用正己烷-二氯甲烷(1:1,V/V)提取,经MCX固相萃取柱进一步净化,采用反相高效液相色谱-紫外检测法进行定量分析。饲料中艾司唑仑的检测限为0.1 mg/kg,定量限为0.25 mg/kg。在饲料中添加0.25,0.5,2.5 mg/kg水平的药物回收试验中,平均回收率均在82.8%～105.9%之间,相对标准偏差为1.62%～8.40 %。该方法灵敏、准确,适用于饲料中艾司唑仑含量的分析检测。

Abstract:

A confirmatory method has been developed and validated for the determination of estazolam (EZL) in premix, compound feed and concentrate feed using high performance liquid chromatography(HPLC). The analyte was extracted from feeds using hexane-dichloromethane (1:1, V/V), and then the sample extracts were purified by MCX solid-phase extraction. The analyte was analyzed by HPLC-UV. The limit of detection was 0.1 mg/kg for EZL, with quantification limit of 0.25 mg/kg. Recoveries were in the range 82.8% to 105.9% from feeds fortified at the 0.25, 0.5, 2.5 mg/kg levels, and the mean intra-laboratory reproducibility ranged from 1.62% to 8.40% (%R.S.D). The developed method is sensitive and specific for the detection of estazolam in feeds.