摘要
为确证乳酸环丙沙星可溶性粉中的非法添加物,采用高效液相色谱-二极管阵列检测器(HPLC-DAD)的谱库匹配,推断出疑似添加物为甲硝唑,从而建立检测乳酸环丙沙星可溶性粉中违规添加甲硝唑和替硝唑的高效液相色谱法。采用Agilent Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-水(20∶80,V∶V),流速为1.0 mL/min,柱温30℃,用二极管阵列检测器进行扫描,扫描范围为190~400 nm,检测波长为320 nm。该色谱条件下甲硝唑和替硝唑与其他物质峰分离良好。甲硝唑和替硝唑在0.5~100μg/mL浓度范围内线性良好,在2.5 mg/g、5.0及10.0 mg/g 3个添加浓度下,加样回收率为99.5%~100.2%,RSD小于1.5%,检测限为2.5 mg/g。本方法简便快捷、准确度和灵敏度高,能满足非法添加物检测的要求。
Illegal additives in a batch of ciprofloxacin lactate soluble powder were identified. The suspected additive was deduced to be metronidazole by matching the spectrum library of HPLC-DAD. A high performance liquid chromatography method was thus established to detect the illegal addition of metronidazole and tinidazole in soluble ciprofloxacin lactate powder. The Agilent Eclipse XDB-C18 column(250 mm×4.6 mm, 5 μm) was used here. The mobile phase was methanol-water(20∶80, v∶v), the flow rate was at 1.0 mL/min, and the column temperature was set as 30 ℃. The scanning range was within 190 nm-400 nm, and the detection wavelength was at 320 nm. Under these chromatographic conditions, metronidazole and tinidazole were well separated from the other peaks. The linearity of metronidazole and tinidazole was good in the range of 0.5 μg/mL-100 μg/mL. The recovery of metronidazole and tinidazole was 99.5%-100.2%, RSD was less than 1.5%, and the detection limit was 2.5 mg/g at the concentrations of 2.5 mg/g, 5.0 mg/g and 10.0 mg/g, respectively. In short, the method was simple and convenient, efficient, accurate and sensitive, which would meet the requirements for detection of illegal additives.
作者
罗成江
王彬
陈晓林
林仙军
LUO Chengjiang;WANG Bin;CHEN Xiaolin;LIN Xianjun(Zhejiang Province Supervisory Institute of Veterinary Drug and Feed,Hangzhou 311101,China)
出处
《畜牧与兽医》
北大核心
2019年第11期63-66,共4页
Animal Husbandry & Veterinary Medicine
基金
浙江省“三农六方”科技协作项目(CTZB-F180706LWZ-SNY1)
