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

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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).

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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