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0.05~2μg/m L范围内线性关系良好(r^2≥0.9991),检出限(S/N=3)为8.27~10.81μg/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。
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.
作者
张玉娜
丁一
孙欣
万秉纯
王明林
ZHANG Yu-Na DING Yi SkIN Xin WAN Bing-Chun WANG Ming-Lin(Central Laboratory of Qingdao Agricultural University, Qingdao 266109, China Shandong Institute for Food and Drug Control, Jinan 250101, China College of Food Science and Engineering, Shandong Agricultural University, Tai ＇an 271018, China)
出处
《食品安全质量检测学报》
CAS
2016年第11期4562-4568,共7页
Journal of Food Safety and Quality
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
milk
quinolones bactericides
cloud point extraction
high performance liquid chromatography
