猪血浆样品中三氮脒质量浓度的高效液相色谱测定方法的建立  

Development of high performance liquid chromatography for determination of the level of diminazene diaceturate in swine plasma samples

作　　者：赵吉祥[1] 李博[1] 路文华 徐维[1] 韩可可 陈杖榴[1] 陈红[1] 

机构地区：[1]华南农业大学兽医学院国家兽药残留基准实验室,广东广州510642

出　　处：《中国兽医科学》2014年第1期93-97,共5页Chinese Veterinary Science

基　　金：2008年农业部财政项目;2009年农业行业标准制定项目

摘　　要：用乙二胺四乙酸二钠溶液稀释猪血浆样品，用SEP—PAK—C，。固相萃取小柱富集药物，再以含有离子对试剂的乙腈洗脱。以氮气吹干洗脱液，流动相复溶后测定药物的质量浓度。HPLC分析柱为BDSC18，流动相组成为V（乙腈）：V（pH3．2的0．005mol／L辛烷磺酸钠溶液）-30：70，紫外检测波长372nm。猪血浆中三氮脒的质量浓度在0．01～40．0μg／mL范围内可准确定量；血浆中三氮脒的质量浓度为0．05、0．5、10μg／mL时，相对回收率≥89．099，6，批间变异系数在0．81％～4．41％之间。猪血浆中三氮脒的定量限为5ng／mL，检测限为2ng／mL。结果表明，本研究建立的HPLC方法操作简单、重复性和灵敏度好，定量范围宽，适用于检测猪血浆样品中三氮脒的质量浓度。A high performance liquid chromatographic（HPLC） method was developed for determina- tion of diminazene diaceturate in swine plasma. Swine plasma samples were diluted in ethylenediaminetetra- acetic acid disodium solution. Then drug in plasma was concentrated by SEP-PAK-C18 cartridge,and eluted by paired-ion/acetonitrile solution from cartridge. The elution was dried by N2 flow,then redissolved with HPLC mobile phase and detected. A BDS C1 8 column was used upon HPLC analysis. Mobile phase consisted of acetonitrile and 0. 005 mol/L octane sulphonic acid sodium solution as pH 3. 2（30 ： 70,V ： V）. The sample was detected at 372 nm. Determination of drug in plasma,within a range from 0.01 vtg/mL to 40.0 μg/mL was accurately available. Relative recovery was 〉89.09 %, while drug concentration was various of 0.05μg/mL,0.5μg/mL,10μg/mL,and relative standard deviation（RSD） ranged from 0.81% to 4.41%. Limit of quantification（LOQ） of this method was 5 ng/mL and limit of detection（LOD） was 2 ng/mL in plasma. The result showed that the method was easy and good in reproducibility and sensitivity, which could be applied to investigations of pharmacology and toxicology.

关 键 词：三氮脒 猪血浆 高效液相色谱 测定 

分 类 号：S859.7[农业科学—临床兽医学]