超高效液相色谱法测定水产品中3种喹诺酮类药物残留量

提出了应用超高效液相色谱法测定水产品中诺氟沙星、环丙沙星和恩诺沙星等3种喹诺酮类药物残留量的方法。样品采用酸化乙腈提取,减压蒸干后用流动相溶解,经正己烷脱脂。以ACQUITY UPLCTMBEH C18色谱柱为分离柱,以乙腈与甲酸(0.1+99.9)溶液按体积比10比90混合作为流动相,在激发波长280nm、发射波长450nm的条件下进行荧光光度检测。3种药物的线性范围均为1.25～500μg.L-1,检出限(3S/N)均为0.1μg.kg-1,测定下限(10S/N)均为0.3μg.kg-1。以鲳鱼、对虾、河蟹等空白样品为基体做加标回收试验,测得回收率均大于80%。

UHPLC Determination of Residual Amounts of 3 Quinolone Drugs in Aquatic Products

A method of UHPLC for determination of residual amounts of 3 quinolone drugs,including norfloxacin,ciprofloxacin and enrofloxacin in aquatic products was proposed.The sample was extracted with acidified acetonitrile,and the extract was evaporated to dryness under reduced pressure.The residue obtained was dissolved in the mixed solvent of mobile phase,and defatted with n-hexane.The ACQUITY UPLCTM BEH C18 column was used as stationary phase,and a mixture of acetonitrile and formic acid solution(0.1+99.9) mixed in the ratio of 10 to 90(by volume) was used as mobile phase.Fluorimetric detection at the wavelengths of(λex) 280 nm and(λem) 450 nm was adopted.Ranges of linearity found were same between 1.25-500 μg·L-1.Values of detection limit(3S/N) and lower limit of determination(10S/N) for 3 drugs were found same to be 0.1 μg·kg-1 and 0.3 μg·kg-1 respectively.Blank samples of pomfret,prawn and crab were analyzed by this method,and test for recovery was made on these matrixes by standard addition method,giving results of over 80%.