浊点萃取-高效液相色谱法检测牛奶中的 喹诺酮类抗生素

Detection of quinolones bactericides in milk by cloud point extraction and high performance liquid chromatography

中文关键词:  牛奶  喹诺酮类抗生素  浊点萃取技术  高效液相色谱法

英文关键词:milk  quinolones bactericides  cloud point extraction  high performance liquid chromatography

中文摘要:

      目的 建立浊点萃取-高效液相色谱(紫外检测器)技术检测牛奶中6种喹诺酮类药物的分析方法。方法 牛奶样品采用冰乙酸和无水硫酸钠破乳, 经 Tween 20表面活性剂萃取后, 加入浓氨水、正丁醇、无水硫酸钠, 在50 ℃水浴锅中进行平衡分离, 将分离出的水相去除, 表面活性剂相进高效液相色谱仪检测分析。 结果 6种喹诺酮类药物在0.05~2 μg/mL范围内线性关系良好(r2≥0.9991), 检出限(S/N=3)为8.27~10.81 μg/L。6种喹诺酮类药物在0.05、0.1、0.2 mg/L 3个水平回收率为71.3%~96.8%, 相对标准偏差为1.24%~6.02%, 结论 该方法准确、灵敏, 符合多残留检测和痕量分析的技术要求。

英文摘要:

      Objective To establish a method for the determination of 6 kinds of quinolones bactericides in milk by cloud point extraction (CPE) and high performance liquid chromatography (HPLC) equipped with ultraviolet detector. Methods The milk samples were demulsified by glacial acetic acid and anhydrous sodium sulfate, then extracted by Tween20. The samples were balanced in 50 ℃ water bath for separation after adding concentrated ammonia, n-butyl alcohol, and anhydrous sodium sulfate. Aqueous phase was removed and surfactant phase was detected by HPLC. Results Under the optimum conditions, good linear relationships were obtained in the range of 0.05~2 μg/mL with correlation coefficients (r2) ≥0.9991, and the limits of detection (S/N=3) were 8.27~10.81 μg/L. The average recoveries at 3 different spiked levels of 0.05, 0.1 and 0.2 μg/mL were 71.3%~96.8%, with relative standard deviations (RSDs) of 1.24%~6.02%. Conclusion This method is accurate and sensitive, which can meet the requirements of multiple residues determination.