高效毛细管电泳法检测牛奶中的青霉素中间体以及3种青霉素类药物

Determination of penicillin intermediate and three penicillins in milk by high performance capillary electrophoresis

建立了高效毛细管电泳(HPCE)同时检测牛奶中青霉素类抗生素中间体6-氨基青霉烷酸(6-APA)以及3种青霉素类药物青霉素钾(PEN)、氨苄青霉素(AMP)和阿莫西林(AMO)的方法。利用正交实验设计,对HPCE中的缓冲液离子浓度和pH值、分离电压、分离温度等分离条件进行了优化。结果表明:在采用40 mmol/L磷酸二氢钾-20 mmo l/L硼砂缓冲体系(pH 7.8)、分离电压为28 kV、分离温度为30℃的电泳条件下,4.5 min内可以实现上述4种青霉素类药物的快速分离检测。各组分在1.56～100 mg/L范围内有良好的线性,相关系数(r 2)为0.997 9～0.999 8,加标回收率为84.91%～96.72%,相对标准偏差(RSDs)为1.11%～9.11%(n=6)。该方法简便、快速,可以应用于市售牛奶中4种青霉素类药物的快速检测。

A high performance capillary electrophoresis（HPCE） method was developed for the simultaneous determination of penicillin intermediate and penicillins in milk,including 6-amino-penicillanic acid（6-APA）,penicillin G（PEN）,ampicillin（AMP） and amoxicillin（AMO）.The main parameters including the ion concentration and pH value of running buffer,separation voltage and column temperature were optimized systematically by orthogonal test.The four penicillins（PENs） were baseline separated within 4.5 min with the running buffer of 40 mmol/L potassium dihydrogen phosphate-20 mmol/L borax solution（pH 7.8）,separation voltage of 28 kV and column temperature of 30 ℃.The calibration curves showed good linearity in the range of 1.56-100 mg/L,and the correlation coefficients（r^2） were between 0.997 9 and 0.999 8.The average recoveries at three spiked levels were in the range of 84.91%-96.72% with acceptable relative standard deviations（RSDs） of 1.11%-9.11%.The method is simple,fast,accurate and suitable for the determination of penicillins in real samples.