未衍生高效液相法测定烤鳗和活鳗中噁喹酸的残留量

 研究了快速测定烤鳗和活鳗中口恶 喹酸残留的高效液相方法。捣碎后的样品用二氯甲烷提取 ,提取液浓缩后再用一定量的流动相溶解残渣 ,并用正己烷去除杂质 ,然后进行高效液相分离及荧光检测。口恶喹酸的最低检出限为 0 0 1mg/kg ,标准添加回收率大于 80 % ,相对标准偏差小于 3 8%。

Determination of Oxolinic Acid Residues in Baked and Fresh Eels by High Performance Liquid Chromatography Without Derivatization

A method for rapid determination of oxolinic acid residues in baked eels and fresh eels by high performance liquid chromatography without derivatization was studied. The samples were triturated, and extracted with methylene dichloride. The extracted solutions were evaporated to dryness, and then was dissolved by using the mobil phase. The solutions were cleaned-up by partition with n-hexane before analysis. The components were analysed on a Nova-Pak C18 column (150 mm x 3.9 mm i.d., 5 microm), with methanol-diluted phosphoric acid (pH 2.5) (40:60, V/V) as the mobile phose at a flow rate of 0.8 mL/min and detected by a fluorescence detector at the excitation wavelength (lambdaex) 254 nm and the emission wavelength (lambdaem) 375 nm. The detection limit was 0.01 mg/kg (S/N = 3). The recoveries were over 80 %, and the relative standard deviations (RSDs) were less than 3.8%.