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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

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【作者】 赵吉祥李博路文华徐维韩可可陈杖榴陈红

【Author】 ZHAO Ji-xiang;LI Bo;LU Wen-hua;XU Wei;HAN Ke-ke;CHEN Zhang-liu;CHEN Hong;College of Veterinary Medicine,South China Agricultural University/National Reference Laboratory of Veterinary Drug Residues;

【机构】 华南农业大学兽医学院 国家兽药残留基准实验室

【摘要】 用乙二胺四乙酸二钠溶液稀释猪血浆样品,用SEP-PAK-C18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BDS C18,流动相组成为V(乙腈)∶V(pH 3.2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≥89.09%,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。

【Abstract】 A high performance liquid chromatographic(HPLC)method was developed for determination of diminazene diaceturate in swine plasma.Swine plasma samples were diluted in ethylenediaminetetraacetic 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 C18 column was used upon HPLC analysis.Mobile phase consisted of acetonitrile and 0.005mol/L octane sulphonic acid sodium solution as pH 3.2(30∶70,V∶V).The sample was detected at 372nm.Determination of drug in plasma,within a range from 0.01μg/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 5ng/mL and limit of detection(LOD)was 2ng/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.

【基金】 2008年农业部财政项目;2009年农业行业标准制定项目
  • 【文献出处】 中国兽医科学 ,Chinese Veterinary Science , 编辑部邮箱 ,2014年01期
  • 【分类号】S859.7
  • 【被引频次】5
  • 【下载频次】125
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