色谱

色谱 ›› 2012, Vol. 30 ›› Issue (10): 1021-1025.DOI: 10.3724/SP.J.1123.2012.08016

• 专栏 • 上一篇    下一篇

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

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*   

  1. 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
  • 收稿日期:2012-08-14 修回日期:2012-08-24 出版日期:2012-10-28 发布日期:2012-10-17
  • 通讯作者: 赵华,副教授,主要从事分析化学及体内药物分析研究. E-mail: zhaohua.cq@sohu.com.
  • 基金资助:

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

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

YOU Lina1, LI Xianliang2,3, XI Cunxian2,3, TANG Bobin2,3, WANG Guomin2,3, ZHANG Lei2,3, YUAN Zhongzhen1, ZHAO Hua1*   

  1. 1. College of Pharmacy, Chongqing Medical University, Chongqing 400016, China; 2. Chongqing Entry-Exit Inspection and Quarantine Bureau, Chongqing 400020, China; 3. Chongqing Engineering Technology Research Center of Import and Export Food Safety, Chongqing 400020, China
  • Received:2012-08-14 Revised:2012-08-24 Online:2012-10-28 Published:2012-10-17

PDF

415

被引次数

32

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 Eclipse XDB-C18(150 mm×4.6 mm, 3.5 μm);流动相: 甲醇-乙腈-水(50:15:35, v/v/v);流速: 1.0 mL/min;检测波长: 270 nm。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)≥0.9998,检出限(LOD,S/N≥3)为1.0 μg/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。

关键词: 高效液相色谱法, 鸡蛋, 免疫亲和柱, 玉米赤霉醇, 玉米赤霉酮, 玉米赤霉烯醇, 玉米赤霉烯酮

Abstract: 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.

Key words: eggs, immunoaffinity column, zearalanone, zearalenol, zearalenone, zeranol, high performance liquid chromatography (HPLC)