咪唑类离子液体用于猪肉中喹诺酮类抗生素高效液相色谱检测方法建立.docVIP

咪唑类离子液体用于猪肉中喹诺酮类抗生素高效液相色谱检测方法建立 　　摘 要：建立以咪唑类离子液体为高效液相色谱流动相添加剂检测猪肉中氟喹诺酮类抗生素的方法。采用C18反相色谱柱和紫外检测方法，对流动相中离子液体溶液的pH值及流动相配比进行优化，同时对方法进行可行性评价。结果表明：当流动相中离子液体溶液的pH值为2.40，离子液体溶液与乙腈的配比为88∶12（V/V）时，诺氟沙星和环丙沙星能够实现基线分离，且分离效果较好。在此条件下，诺氟沙星和环丙沙星在质量浓度为0.05～80.00 μg/mL范围内的检出限分别为0.014 μg/mL和0.022 μg/mL，且线性关系良好（R20.999 0）；2 种物质的保留时间和峰面积的日内及日间（3 d）精密度均小于1.50%，符合测定要求；在猪肉样品中添加2、5、10 mg/kg的诺氟沙星和环丙沙星标准品，其固相萃取回收率在95.3%～102.0%之间，表明方法精密度较好，可用于猪肉中喹诺酮类抗生素的测定。 　　关键词：咪唑类离子液体；高效液相色谱法；流动相添加剂；猪肉；氟喹诺酮类抗生素 　　Establishment of High Performance Liquid Chromatography Method for Determination of Quinolones in Pork 　　Using Imidazolium-Based Ionic Liquids as Mobile Phase Additives 　　TIAN Jing， XIN Keqi， ZHU Zidong， NIU Shubin* 　　（The Experimental Teaching Center of Traditional Chinese Medicine and Biotechnology， Beijing City University， Beijing 100094， China） 　　Abstract： A reversed-phase high performance liquid chromatographic （RP-HPLC） method was established for the determination of quinolones in pork by using imidazolium-based ionic liquids as mobile phase additives. The chromatographic separation of quinolones was performed on a C18 column before ultraviolet detection. The effects of the pH value of ionic liquid and mobile phase composition on the analysis were investigated and optimized. The performance of the method was evaluated in terms of linear range， detection limit and reproducibility. Good baseline separation of norfloxacin and ciprofloxacin was achieved using imidazolium aqueous solution （pH 2.40）-acetonitrile （88：12， V/V） as the mobile phase. Under this condition， the calibration curves of norfloxacin and ciprofloxacin showed a good linearity in the concentration range of 0.05?80.00 μg/mL with R2 greater than 0.999 0， and the detection limits were 0.014 and 　　0.022 μg/mL， respectively. The intra-day and inter-day precision of migration time and peak area were less than 1.50% for both quinolones， which met the analytical requirements. The average recoveries at three spiked levels （2， 5， 10