高效液相色谱内标法测定鸡蛋中氯羟吡啶的残留量  

Determination of clopidol residue in eggs by liquid chromatography internal standard method

作　　者：方奕珊[1] 李来生[1] 陈红[1] 张杨[1] 

机构地区：[1]南昌大学分析测试中心,江西南昌330047

出　　处：《南昌大学学报（理科版）》2011年第5期453-456,共4页Journal of Nanchang University(Natural Science)

基　　金：江西省自然科学基金资助项目(2010GZH0089);江西省教育厅科技基金资助项目(GJJ11274)

摘　　要：以4-二甲氨吡啶为内标,发展了一种高效液相色谱法,用于快速测定鸡蛋中氯羟吡啶的残留量。鸡蛋样品中的氯羟吡啶经乙腈匀浆提取,然后用碱性氧化铝柱富集,甲醇洗脱液浓缩后用流动相溶解残渣,0.45μm滤膜过滤后进样分析。色谱柱采用Platisil-C18柱(4.6mm×250mm,5μm),流动相为0.05mol.L-1甲酸铵-乙腈(85:15,v/v,pH 6.4),流速为0.8mL.min-1,二极管阵列定量检测波长为267nm,柱温25℃,进样量20μL。氯羟吡啶在0.5～80μg.mL-1范围内呈现良好的线性关系,线性方程为Y=0.254 4 X+0.703 9,相关系数为0.999 6。3个不同水平的标准添加平均回收率分别为85.3%,88.2%和83.7%,相对标准偏差≤2.25%(n=4)。最低检出限为1.8mg.kg-1。该方法快速、简便、准确、重现性好,适用于鸡蛋中兽药氯羟吡啶残留量的快速检测。The high performance liquid chromatography（HPLC） method for determination of clopidol in eggs was developed.The clopidol residue in eggs was extracted from acetonitrile with the following procedure：firstly purified by alumina SPE cartridge with methanol as eluent,then concentrated the eluent with the mobile phase dissolved residues,finally filtered and analyzed by platisil C18 column（4.6 mm×250 mm,5 μm） and 4-dimethylamino pyridine as internal standard,with UV detector at 267 nm and 0.05 mol·L-1 ammonium formate-acetonitrile（85：15,v/v） as mobile phase in room temperature.A 20-μL volume of samples was injected for chromatographic analysis.The results illustrated that there was good linear relationship（r=0.999 6） between X and Y when clopidol concentration was in the range of 0.5 to 80 μg·mL-1,with a linear equation Y=0.254 4X＋0.703 9.The average coefficient of recoveries at three different levels were 85.3%,88.2%,83.7% with RSD≤2.25%,respectively.The detection limition of clopidol in eggs was 5 μg·kg-1.The method is rapid,simple,accurate and reproducible,which is applicable to detect the veterinary drugs clopidol residues in eggs fast.

关 键 词：高效液相色谱法 氯羟吡啶 鸡蛋 残留量 内标法 

分 类 号：O657.7[理学—分析化学]