高效液相色谱法分析氰戊菊酯微乳剂、水乳剂

HPLC Analysis of the Water Emulsions and Microemulsion of Fenvalerate

采用异丙醇提取微乳剂型和水乳剂型氰戊菊酯样品中的有效成分氰戊菊酯,以正相高效液相色谱法测定氰戊菊酯含量.样品提取后用流动相定容,经0.45 μm 针式有机滤膜过滤,通过lnertsil SIL–100A 硅胶色谱柱进行分离,以正己烷–乙酸乙酯（体积98∶2）作为流动相,流量为2 mL/min,紫外检测波长为254 nm,柱温为30℃,外标法定量.氰戊菊酯的质量浓度在0.8～4.0 mg/mL 范围内与色谱峰面积呈良好的线性关系,相关系数r=0.999 6,检出限为10 μg/mL.在3 个添加水平下,样品的加标回收率在89.2%～98.6% 之间,测定结果的相对标准偏差均小于3%（n=6）.该方法快速、简单、准确,可用于批量样品的氰戊菊酯成分定量定性检验.

Isopropyl alcohol was used to extract the active ingredient fenvalerate in water emulsions and microemulsionfenvalerate sample, fenvalerate content was determined by normal phase high performance liquid chromatography.After being extracted, the sample solution was mixed with mobile phase, filted with organic needle 0.45μm membranefilter, then separated by silica gel column. Hexane–ethyl acetate （volume rate was 98∶2） was used as mobile phase withflow rate of 2 mL/min, UV wavelength was at 254 nm, column temperature was 30 ℃ .External standard method wasused. Fenvalerate concentration was linear with the chromatographic peak area in the range of 0.8–4.0 mg/mL, and thecorrelation coefficient r was 0.999 6,the detection limit was 10 μg/mL. In the three spiked levels, recoveries were89.2%–98.6%,and the relative standard deviation of detection results was less than 3% （n=6）. The method is rapid,simpleand accurate for fenvalerate quantitative and qualitative detection of the bulk sample.