色谱 ›› 2018, Vol. 36 ›› Issue (3): 292-298.DOI: 10.3724/SP.J.1123.2017.11049

• 研究论文 • 上一篇    下一篇

新型分散液液微萃取-高效液相色谱法检测盐酸利多卡因注射液中2,6-二甲基苯胺杂质

王璇璇, 李潇, 肖玉秀   

  1. 组合生物合成与新药发现教育部重点实验室, 武汉大学药学院, 湖北 武汉 430071
  • 收稿日期:2017-11-24 出版日期:2018-03-08 发布日期:2018-04-04
  • 通讯作者: 肖玉秀,Tel:(027)68759892,E-mail:yuxiuxiao2011@whu.edu.cn
  • 基金资助:

    国家自然科学基金面上项目(81673394,81373045);湖北省自然科学基金重点项目(2015CFA139).

A novel dispersive liquid-liquid microextraction method with high performance liquid chromatography for detection of 2,6-dimethylaniline in lidocaine hydrochloride injection

WANG Xuanxuan, LI Xiao, XIAO Yuxiu   

  1. Key Laboratory of Combinatorial Biosynthesis and Drug Discovery(Ministry of Education), School of Pharmaceutical Sciences, Wuhan University, Wuhan 430071, China
  • Received:2017-11-24 Online:2018-03-08 Published:2018-04-04
  • Supported by:

    National Natural Science Foundation of China (Nos. 81673394, 81373045); Provincial Natural Science Foundation of Hubei of China (No. 2015CFA139).

摘要:

以正辛醇为萃取剂,六氟异丙醇(HFIP)为分散剂、正辛醇的自组装诱导剂和密度调节剂,建立了基于HFIP-正辛醇超分子溶剂(SUPRAS)的新型分散液液微萃取(DLLME)方法;应用该萃取方法和HPLC-UV法检测了盐酸利多卡因注射液中的2,6-二甲基苯胺(2,6-DMA)杂质。HFIP-正辛醇SUPRAS为反向胶束聚集体结构,且位于体系的下层,因此有利于萃取富集极性较大的2,6-DMA,且可简化萃取操作。在最佳萃取条件(0.4%(v/v)正辛醇,5%(v/v) HFIP,涡旋3 s,静置3 min,以3000 r/min离心3 min,样品溶液pH 9)下,2,6-DMA的富集因子约为63。在1~100 μg/L范围内方法的线性关系良好(R=0.9989),检出限为0.33 μg/L,日内、日间精密度均不高于2.5%,回收率为93.9%~100.8%。新型DLLME方法简便、快速、高效、环保,其与HPLC-UV法结合可定量检测盐酸利多卡因注射液中的2,6-DMA。

关键词: 2, 6-二甲基苯胺, 超分子溶剂, 分散液液微萃取, 高效液相色谱, 六氟异丙醇, 盐酸利多卡因注射液, 正辛醇

Abstract:

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). n-Octanol was selected as extraction solvent while HFIP was served as dispersing agent, self-assembly inducer of n-octanol as well as density-regulating agent of n-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) n-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 (R=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 (n=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.

Key words: n-octanol, 2,6-dimethylaniline (2,6-DMA), dispersive liquid-liquid microextraction (DLLME), hexafluoroisopropanol, high performance liquid chromatography (HPLC), lidocaine hydrochloride injection, supramolecular solvent

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