色谱

色谱

• 研究论文 • 上一篇    下一篇

固相萃取-胶束电动色谱法测定牛奶中的4种β-内酰胺类抗生素

张琦,叶能胜,谷学新,郝晓丽,刘妮   

  1. Department of Chemistry, Capital Normal University, Beijing 100048, China
  • 收稿日期:2008-06-17 修回日期:2008-09-17 出版日期:2008-11-30 发布日期:1983-06-25
  • 通讯作者: 谷学新
  • 基金资助:
    北京市教委科技发展项目(No. KM200710028010)

Simultaneous determination of four β-lactam antibiotics in milk by solid-phase extraction-micellar electrokinetic chromatography

ZHANG Qi, YE Nengsheng, GU Xuexin, HAO Xiaoli, LIU Ni   

  1. Department of Chemistry, Capital Normal University, Beijing 100048, China
  • Received:2008-06-17 Revised:2008-09-17 Online:2008-11-30 Published:1983-06-25
  • Contact: GU Xuexin

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摘要： 建立了同时分离检测牛奶中的氨苄西林、阿莫西林、青霉素V和头孢氨苄4种β-内酰胺类抗生素的固相萃取-胶束电动色谱法。牛奶样品经沉淀蛋白后,采用HLB固相萃取柱净化浓缩;以含十二烷基硫酸钠(SDS)的磷酸盐为缓冲液,胶束电动色谱分离,210 nm波长下检测。分离电压为18 kV,于9 min内达到基线分离。各组分在0.5～20 mg/L范围内呈良好的线性关系,相关系数(r2)为0.9943～0.9976;检出限为0.16～0.20 mg/L;除了阿莫西林外,回收率均大于70%。该方法准确可靠,重复性好,灵敏度高,可以用于牛奶中β-内酰胺类抗生素的定量检测。

关键词: β-内酰胺类抗生素, 固相萃取, 胶束电动色谱, 牛奶

Abstract: A solid-phase extraction (SPE)-micellar electrokinetic chromatography (MEKC) method was developed for the simultaneous determination of four β-lactam antibiotics (ampicillin, amoxicillin, penicillin V and cephalexin) in spiked milk samples. The milk samples were extracted by SPE after protein precipitation. The analysis was performed by MEKC at 18 kV with phosphate buffer containing sodium dodecyl sulfate (SDS) and the detection was carried out at 210 nm. The four antibiotics could be baseline-separated less than 9 min. The linearities in 0.5-20 mg/L could be constructed with the correlation coefficients between 0.9943-0.9976, and the limits of detection were 0.16-0.20 mg/L. The average recoveries of antibiotics from milk were over 70% except amoxicillin. The method is sensitive, specific and easy for the determination of β-lactam antibiotic residues in milk.

Key words: micellar electrokinetic chromatography (MEKC), milk , β-lactam antibiotics, solid-phase extraction (SPE)