超分子溶剂液液微萃取-超高效液相色谱法检测萘敏维滴眼液中的防腐剂尼泊金乙酯

Determination of preservative ethylparaben in naphazoline eye drops by supramolecular solvent-based liquid-liquid microextraction with ultra-performance liquid chromatography

目的 建立了超分子溶剂液液微萃取联用超高效液相色谱(ultra performance liquid chromatography, UPLC)法检测萘敏维滴眼液中的防腐剂尼泊金乙酯(ethylparaben, EP)。方法 以正辛醇为萃取剂、水和六氟异丙醇(hexafluoroisopropanol, HFIP)为分散剂组成的新型萃取剂位于溶剂体系下层,有利于实现对极性较大的EP的萃取。结果 在最佳萃取条件(2%正辛醇、6%HFIP、涡旋3 min、离心2 min)下,EP的萃取率最高。EP在0.01~20 mg/L范围内方法的线性关系良好(R~2=0.999 1),最小检出量为1.2μg/L,日内精密度为4.82%,日间精密度为3.21%。结论 结合UPLC法可定量检测萘敏维滴眼液中的防腐剂EP,方法绿色环保,处理过程简单快速。

Objective Supramolecular Solvents liquid-liquid microextraction combined with ultra performance liquid chromatography(UPLC) method was developed for the determination of preservative ethylparaben in naphazoline eye drops. Methods The new supramolecular solvent which was prepared with n-octanol as extraction solvent, water and Hexafluoroisopropanol(HFIP) as dispersing agent, was located in the bottom phase of the solvent system after phase separation, which could facilitate the efficient extraction and enrichment of polar ethylparaben. Results Under optimum condition(2% n-octanol, 6% HFIP, vortex for 3 min, centrifugation for 2 min, the extraction rate of ethylparaben was the highest. The method showed good linearity for quantitative detection of ethylparaben in the range of 0.01〜20 mg/L(R^(2)=0.9991). The limit of detection was 1.2 μg/L, the intra-day precision was 4.82% and inter-day precision was 3.21%. Conclusion The method was suitable for the accurate quantitative determination of preservative ethylparaben in naphazoline eye drops with advantage of green chemistry, simplicity, rapidness.