Citation: WANG Xuanxuan, LI Xiao, XIAO Yuxiu. A novel dispersive liquid-liquid microextraction method with high performance liquid chromatography for detection of 2,6-dimethylaniline in lidocaine hydrochloride injection[J]. Chinese Journal of Chromatography, ;2018, 36(3): 292-298. doi: 10.3724/SP.J.1123.2017.11049 shu

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

Key Laboratory of Combinatorial Biosynthesis and Drug Discovery(Ministry of Education), School of Pharmaceutical Sciences, Wuhan University, Wuhan 430071, China

Received Date: 24 November 2017

Fund Project: National Natural Science Foundation of China (Nos. 81673394, 81373045)

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.
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