免疫亲和柱净化-高效液相色谱法同时检测鸡蛋中6种玉米赤霉醇类化合物残留量  

Simultaneous determination of residues of six zeranols in eggs by high performance liquid chromatography with immunoaffinity cleanup column

作　　者：游丽娜[1] 李贤良[2,3] 郗存显[2,3] 唐柏彬[2,3] 王国民[2,3] 张雷[2,3] 袁中珍[1] 赵华[1] 

机构地区：[1]重庆医科大学药学院,重庆400016 [2]重庆出入境检验检疫局,重庆400020 [3]重庆市进出口食品安全工程技术研究中心,重庆400020

出　　处：《色谱》2012年第10期1021-1025,共5页Chinese Journal of Chromatography

基　　金：科技部质检公益项目(201210086);国家认监委检验检疫行业标准项目(2011B138)

摘　　要：建立了鸡蛋中6种玉米赤霉醇类化合物(α-玉米赤霉醇、β-玉米赤霉醇、α-玉米赤霉烯醇、β-玉米赤霉烯醇、玉米赤霉酮和玉米赤霉烯酮)残留量的免疫亲和柱净化-高效液相色谱检测方法。样品酶解后用叔丁基甲醚提取、氢氧化钠反萃取,经免疫亲和柱富集和净化后,采用高效液相色谱-紫外检测器进行测定。色谱柱:Agilent EclipseXDB-C18(150 mm×4.6 mm,3.5μm);流动相:甲醇-乙腈-水(50∶15∶35,v/v/v);流速:1.0 mL/min;检测波长:270nm。结果表明,6种目标物在0.01～0.2 mg/L范围内线性关系良好,相关系数(r)≥0.999 8,检出限(LOD,S/N≥3)为1.0μg/kg,平均回收率为73.2%～95.7%,相对标准偏差小于8%。该方法灵敏度高、重现性好,适用于鸡蛋样品中痕量玉米赤霉醇类药物残留的测定。An immunoaffinity cleanup-high performance liquid chromatography（IAC-HPLC） method was established for the simultaneous determination of residues of six zeranols（α-zeranol,β-zeranol,α-zearalenol,β-zearalenol,zearalanone and zearalenone） in eggs.The enzymolyzed samples were extracted with methyl tert-butyl ether,and subsequently reextracted with a sodium hydroxide solution.After the pH value was adjusted to 7,the extract was cleaned up on an immunoaffinity column.The chromatographic separation was performed on an Agilent Eclipse XDB-C18 column（150 mm×4.6 mm,3.5 μm） using methanol-acetonitrile-water（50∶15∶35,v/v/v） as the mobile phase at a flow rate of 1.0 mL/min and ultraviolet（UV） detection at 270 nm.The six zeranols had good linear relationships in the range of 0.01-0.2 mg/L with the correlation coefficients not less than 0.9998;the recoveries of six target compounds at different spiked levels ranged from 73.2% to 95.7% and the relative standard deviations were less than 8%.The limit of detection（S/N≥3） was 1.0 μg/kg for each zeranol.The method is stable,reliable and accurate,and can be used for the determination of trace residues of the six zeranols in eggs.

关 键 词：高效液相色谱法 免疫亲和柱 玉米赤霉醇 玉米赤霉烯醇 玉米赤霉酮 玉米赤霉烯酮 鸡蛋 

分 类 号：O658[理学—分析化学]