提出了高效液相色谱-荧光光度检测尿液中溴鼠录.尿液经磷酸酸化至pH 2.0并在LC-18固相萃取小柱上富集、净化,分取10.0 μL试样溶液进行高效液相色谱测定.用XDB C18柱(150 mm×2.1 mm,5 μm)为固定相,以甲醇及稀乙酸溶液(2+998)以88比12的比例混合后作为流动相,在激发波长为270 nm,发射波长为376 nm的条件下进行荧光光度检测.结果表明:溴鼠灵在0.05~10.0 mg·L-1范围内呈线性关系,方法的回收率在79.8%~97.0%之间,相对标准偏差在4.0%~4.9%之间,测定限为0.07 mg·L-1.

A method of HPLC determination of brodifacoum (BDFC) in urine with FPD was proposed. Urine sample was acidified with H3PO4 to pH 2.0 and treated by SPE on LC-18 micro-column. Brodifacoum was eluted from the column with eluant containing methanol and methyl tert. butyl ether mixed in the ratio of 1 to 9. The eluate obtained was blown to dryness with nitrogen gas,and the residue was dissolved with 1.0 mL of methanol,from which 10.0 μL was aliquoted and introduced into the instrument for HPLC determination. Chromatographic column of XDB-C18 (150 mm×2.1 mm,5 μm) was used as the stationary phase,and a mixed solution of methanol and dil. acetic acid solution (2+998),mixed in the ratio of 88 to 12,was used as the mobile phase. Fluorophotometric detection at the wavelengths of (λex) 270 nm and (λem) 376 nm was adopted. Linearity range of the method was found in the range of 0.05-10.0 mg·L-1 of BDFC. Determination limit (S/N=10) of the method was found to be 0.07 mg·L-1. Values of recovery and RSD (n=6) found were in the ranges of 79.8%-97.0% and 4.0%-4.9% respectively.