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采用离子液体(1-丁基-3-甲基咪唑六氟磷酸盐)建立一种分散液-液微萃取技术,结合高效液相色谱法(HPLC)用于检测牛奶中的青霉素V和氯唑西林。样品处理条件为:提取液为0.02 mol/L的磷酸缓冲液5 mL,离子液体60μL,分散剂为1 mL乙腈/甲酸(99.8∶0.2,v/v),提取时间1.5 min,离心8 min。结果显示该方法对牛奶中青霉素V和氯唑西林的富集倍数分别为35倍和82倍。然后采用HPLC方法对青霉素V和氯唑西林进行检测,检测限分别为0.2和1.5 ng/mL。两种药物在空白牛奶中的添加回收率在84.1%~96.7%之间,变异系数小于4.9%。通过对未知牛奶样品进行检测,证明该方法可以作为一种简单、灵敏、准确的工具用于检测牛奶中的两种药物。
A liquid-liquid microextraction technique was developed using ionic liquid (1-butyl-3-methylimidazolium hexafluorophosphate). HPLC was used to detect penicillin V and chlorzole in milk Xilin. The sample was treated with 5 mL of 0.02 mol / L phosphate buffer, 60 μL of ionic liquid, 1 mL of acetonitrile / formic acid (99.8: 0.2, v / v) as dispersant, 1.5 min of extraction time and 8 min of centrifugation. The results showed that the enrichment fold of penicillin V and cloxacillin in milk was 35 times and 82 times respectively. The HPLC method was used to detect penicillin V and cloxacillin with the detection limits of 0.2 and 1.5 ng / mL, respectively. The recoveries of two drugs in blank milk ranged from 84.1% to 96.7%, and the coefficient of variation was less than 4.9%. By testing unknown milk samples, the method proved to be a simple, sensitive and accurate tool for detecting two drugs in milk.