Wang Xuanxuan, Li Xiao, Xiao Yuxiu
Key Laboratory of Combinatorial Biosynthesis and Drug Discovery(Ministry of Education), School of Pharmaceutical Sciences, Wuhan University, Wuhan 430071, China.
Key Laboratory of Combinatorial Biosynthesis and Drug Discovery(Ministry of Education), School of Pharmaceutical Sciences, Wuhan University, Wuhan 430071,
Se Pu. 2018 Mar 8;36(3):292-298. doi: 10.3724/SP.J.1123.2017.11049.
A novel hexafluoroisopropanol (HFIP)-octanol supramolecular solvent (SUPRAS) based dispersive liquid-liquid microextraction (DLLME) method was developed for the determination of 2,6-dimethylaniline (2,6-DMA) in lidocaine hydrochloride injection coupled with high performance liquid chromatography-ultraviolet detection (HPLC-UV). -Octanol was selected as extraction solvent while HFIP was served as dispersing agent, self-assembly inducer of -octanol as well as density-regulating agent of -octanol. The HFIP-octanol SUPRAS displays reverse micellar aggregate structures (2-6 μm) with hydrophilic inner cores and is located in the bottom phase of the system after phase separation, which not only facilitates the efficient extraction and enrichment of polar 2,6-DMA, but also simplifies the extraction process. Several parameters influencing the extraction efficiency of 2,6-DMA were investigated and optimized. Under optimum conditions (0.4%(v/v) -octanol, 5% (v/v) HFIP, vortex for 3 s at 60 W, standing for 3 min, centrifugation for 3 min at 3000 r/min, sample solution pH 9), the novel DLLME-HPLC method shows good linearity for quantitative detection of 2,6-DMA in the range of 1-100 μg/L (=0.9989). The limit of detection (LOD) was 0.33 μg/L. The enrichment factor (EF) reached about 63. Intra-day and inter-day precisions (=3) were all below 2.5%. The recoveries were from 93.9% to 100.8%. The results demonstrate that the novel DLLME-HPLC method is suitable for the accurate quantitative determination of 2,6-DMA in lidocaine hydrochloride injection with advantages of simplicity, rapidness, high efficiency and environmental friendliness, and may own high potential in future prospects.
建立了一种基于新型六氟异丙醇(HFIP)-辛醇超分子溶剂(SUPRAS)的分散液液微萃取(DLLME)方法,用于盐酸利多卡因注射液中2,6-二甲基苯胺(2,6-DMA)的测定,并结合高效液相色谱-紫外检测(HPLC-UV)。选择辛醇作为萃取溶剂,而HFIP作为分散剂、辛醇的自组装诱导剂以及辛醇的密度调节剂。HFIP-辛醇SUPRAS呈现出具有亲水性内核的反胶束聚集体结构(2-6μm),相分离后位于体系的下层,这不仅有利于极性2,6-DMA的高效萃取和富集,还简化了萃取过程。研究并优化了影响2,6-DMA萃取效率的几个参数。在最佳条件下(0.4%(v/v)辛醇、5%(v/v)HFIP、60W下涡旋3s、静置3min、3000r/min离心3min、样品溶液pH9),该新型DLLME-HPLC方法对2,6-DMA的定量检测在1-100μg/L范围内具有良好的线性(r = 0.9989)。检测限(LOD)为0.33μg/L。富集因子(EF)约为63。日内和日间精密度(n = 3)均低于2.5%。回收率为93.9%至100.8%。结果表明,该新型DLLME-HPLC方法适用于盐酸利多卡因注射液中2,6-DMA的准确定量测定,具有简单、快速、高效和环境友好的优点,未来可能具有很大的潜力。