Journal
JOURNAL OF SEPARATION SCIENCE
Volume 35, Issue 1, Pages 145-152Publisher
WILEY PERIODICALS, INC
DOI: 10.1002/jssc.201100729
Keywords
Emodin; Ionic liquid dispersive liquid-liquid microextraction; Organic solvent dispersive liquid-liquid microextraction; Metabolite
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Funding
- National Nature Science Foundation of China [81041084]
- Nature Science Foundation of Shanxi Province, China [2011011035-2]
- Higher Learning Institutions of Shanxi Province, China
- Innovation Foundation of Shanxi Medical University, China
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In this paper, two methods based on organic solvent dispersive liquid-liquid microextraction (OS-DLLME) and ionic liquid dispersive liquid-liquid microextraction (IL-DLLME) coupled with high-performance liquid chromatography have been critically compared for analyzing emodin and its metabolites (aloe-emodin, anthraquinone-2-carboxylic acid, rhein, danthron, chrysophanol and physcion) in urine samples. Several important parameters influencing the extraction recoveries of DLLME were carefully optimized. Under optimal conditions, the enrichment factors (EFs) for emodin and its metabolites by OS-DLLME and IL-DLLME were within the range of 90-295 and 63-192 respectively; the relative standard deviations (RSDs, n = 3) for intra-day and inter-day precision were lower than 7.2 and 8.7% by OS-DLLME, and lower than 5.7 and 6.4% by IL-DLLME; the recoveries of emodin and its metabolites were from 87.1 to 105% for OS-DLLME and from 94.8 to 103% for IL-DLLME, respectively. There were no significant deviations between the two methods for the determination of emodin and its metabolites. From the results of HPLC/UV of urine sample after DLLME, the metabolites aloeemodin, rhein, chrysophanol and physcion were identified by comparing the retention times with the standards. From the results of HPLC/MS, anthraquinone-2-carboxylic acid and danthron as unreported metabolites of emodin were found.
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