高压液相色谱-荧光检测法检测蜂王浆中喹诺酮类药物残留的方法

Determination of Residues of Norfloxacin,Ciprofloxacin and Enrofloxacin in Royal Jelly by High Performance of Liquid Chromatography with Fluorescence Detector

建立了一种高压液相色谱-荧光检测法同时检测蜂王浆中诺氟沙星、环丙沙星和恩诺沙星残留量的方法。采用10 mL PH3.0、0.2 mol/L的三氟乙酸溶液和20 mL乙腈作为提取液,提取液经浓缩、SCX固相萃取小柱净化、4 mL 0.1 mol/L的氢氧化钠溶液洗脱,15%柠檬酸调节pH值,荧光检测器(激发波长280 nm,发射波长450 nm)进行检测。该方法在2~50μg/kg范围内线性关系良好,提取回收率在59%〜91%,方法的检测限为1.0 g/kg。由此可见,该方法检测限低,准确度高,可用于蜂王浆中3种喹诺酮类药物残留的检测。

A HPLC-FD method has been set up to determine simultaneously the residues of Norfloxacin,Ciprofloxacin and Enofloxacin in royal jelly.In the course of study,the extracting solut ions,the clean-up procedures and the chromatography conditions were screened and decided.The 0.2 mol/L TFA(pH3.0)and ACN were used as extracting solution.The SCX SPE column was used to clean up the sample after the extracting solution was concentrated.4 mL of 0.1 mol/L NaOH solution was used to elute the column and 0.2 mL of 15%citric acid was added into elution to adjust the acidity.The excitation wavelength was 280 nm and the emission wavelength was 450 nm.The linear range of method was 2-50μg/kg.The range of recovery rate was 59%-91%.The detection limit was 1.0μg/kg.The method is sensitive and accurate,which is suitable for quantitative analysis of 3 kinds of quinolonesresidues in royal jelly.