食品科学

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免疫亲和柱-高效液相色谱法测定牛奶中氯霉素和玉米赤霉醇及其类似物

姚 佳1,王 昕1,张建新1,*,李贤良2,郗存显2,王国民2,王 雄3,里 南3,果 旗3   

  1. 1.西北农林科技大学食品科学与工程学院,陕西 杨凌 712100;2.重庆出入境检验检疫局,重庆 400020;
    3.北京中检维康技术有限公司,北京 100044
  • 出版日期:2014-09-25 发布日期:2014-09-17
  • 通讯作者: 张建新
  • 基金资助:

    国家质量监督检验检疫局公益性行业科研专项(201210086)

Simultaneous Determination of Residues of Chloramphenicol, Zearalanol and Its Analogs in Milk by High Performance Liquid Chromatography with Immunoaffinity Column

YAO Jia1, WANG Xin1, ZHANG Jian-xin1,*, LI Xian-liang2, XI Cun-xian2, WANG Guo-min2, WANG Xiong3, LI Nan3, GUO Qi3   

  1. 1. College of Food Science and Engineering, Northwest A & F University, Yangling 712100, China; 2. Chongqing Entry-Exit Inspection
    and Quarantine Bureau, Chongqing 400020, China; 3. Clover Technology Group Inc., Beijing 100044, China
  • Online:2014-09-25 Published:2014-09-17
  • Contact: ZHANG Jian-xin

摘要:

建立免疫亲和柱同时净化-高效液相色谱法测定牛奶中氯霉素和玉米赤霉醇及其类似物(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)残留量的方法。样品经免疫亲和柱净化与富集后,用高效液相色谱-紫外检测器检测。采用Cloversil-C18反相柱分离,流动相为乙腈-甲醇-水溶液,检测波长为265 nm。结果表明,牛奶中添加氯霉素和玉米赤霉醇及其类似物的回收率在74%~101%,且相对标准偏差均小于7%。氯霉素的检出限为0.02 μg/L,玉米赤霉醇及其类似物的检出限分别为α-玉米赤霉醇0.03 μg/L、β-玉米赤霉醇0.03 μg/L、α-玉米赤霉烯醇0.03 μg/L、β-玉米赤霉烯醇0.03 μg/L、玉米赤霉酮0.04 μg/L和玉米赤霉烯酮0.05 μg/L。该方法灵敏度高、重复性好,提高了检测速率,可满足牛奶样品中痕量氯霉素和玉米赤霉醇及其类似物残留的测定。

关键词: 牛奶, 氯霉素, 玉米赤霉醇, 免疫亲和柱, 高效液相色谱

Abstract:

An immunoaffinity column cleanup-high performance liquid chromatography (HPLC) method was established for
the simultaneous determination of residues of chloramphenicol, zearalanol and its analogs (α-zeranol, β-zeranol, α-zearalenol,
β-zearalenol, zearalanone, and zearalenone) in milk. Samples were cleaned up and enriched on an immunoaffinity column.
The chromatographic separation was performed on a Cloversil-C18 column using acetonitrile-methanol-water as the mobile
phase and ultraviolet (UV) detection was performed at 265 nm. The recoveries of seven target compounds at different
spiked levels ranged from 74% to 101% and the relative standard deviations were less than 7%. The limits of detection
were 0.02 μg/L for chloramphenicol, 0.03 μg/L for α-zearalanol, β-zearalanol, α-zearalenol, and β-zearalenol, 0.04 μg/L for
zearalanone, and 0.05 μg/L for zearalenone. The proposed method is efficient, stable, reliable and accurate, and can be used
for the determination of trace residues of chloramphenicol, zearalanol and its analogs in milk.

Key words: milk, chloramphenicol, zearalanol, immunoaffinity column, high performance liquid chromatography (HPLC)

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