建立了高效液相色谱-荧光测定蔬菜中4种喹诺酮类抗生素的分析方法。蔬菜样品采用酸化乙腈超声提取,再以正己烷液-液萃取并旋转蒸发浓缩。采用高效液相色谱-荧光检测器,以乙腈/0.086mol/L磷酸(15/85,V/V,用三乙胺调节pH2.5)作为流动相,于激发波长280 nm、发射波长450 nm处对样品进行检测。4种喹诺酮类抗生素在蔬菜中的检测限为0.575~1.538μg/kg,不同浓度加标回收率为64.4%~116.9%。对环境中蔬菜样品进行检测结果表明该方法有效可行且价廉,能够满足日常监测分析要求。
An analytical method for the simultaneous determination of four quinolones in vegetable was developed. Vegetable samples were ultrasonically extracted by aeetonitrile added with hydrochloric acid (125/1,v/v), followed by a double liquid-liquid extraction with N-hexane and enrichment with circumrotating evaporation.Analytes were quantificated by high performance liquid chromatography-fluorimetric detector (HPLC-FLD) at excitation and emission wavelength of 280 nm and 450 nm respectively using acetonitrile/0.086 mol/L phosphoric acid(15/85,v/v) as the mobile phase(adjusted pH value to 2.5 with triethylamine).The detective limits of four quinolones antibiotics in vegetable were obtained from 0.575 to 1.538 μg/kg, and the recoveries were obtained from 64.4 to 111.9%. Application of the method was successfully used to determine four quinolones antibiotics in various vegetables.