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Concentrated of DLLME on anthraquinone compounds in complex samples , enrichment and chromatographic analysis
Author: TianJie
Tutor: BaiXiaoHong
School: Shanxi Medical
Course: Drug analysis
Keywords: DLLME Ionic liquids Anthraquinones compounds Molecular assemblies The organic solvent DLLME Ionic liquids DLLME High Performance Liquid Chromatography Emodin Metabolites Urine samples
CLC: R284
Type: Master's thesis
Year: 2011
Downloads: 75
Quote: 0
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Abstract
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The first part of the Chinese herbal component organic solvents and ionic liquids DLLME method comparison and mechanism of this paper, the ionic liquid DLLME (ionic liquid based dispersive liquid phase microextraction, ILDLPME) mechanism; compared ILDLPME and organic solvent DLLME (organic solvent based dispersive liquid phase microextraction, OSDLPME) in the determination of the similarities and differences in the application of anthraquinone compounds; the DLLME - high performance liquid chromatography determination herbs 6 kinds of free anthraquinones compounds (Aloe emodin, rhein, Dan anthraquinone, emodin, chrysophanol and emodin) content. Optimized experimental conditions of OSDLPME and ILDLPME analyte enrichment factor of 101 to 230 times and between 76 to 181 times; combination of HPLC determination of analyte detection limit, respectively, in the 20 ~ 200pg.ml between -1 and 40 ~ 400pg.ml-1; precision (RSD), respectively, in the range of 3.1% to 10.0% and from 1.3% to 7.0%; herbs analyte recovery rate of 81.7% to 110.7% and from 81.9% to 110.8%. Ordered arrangement of the ionic liquid dispersed in water to form molecular assemblies, analyte extraction. ILDLPME reaches equilibrium faster time, higher precision, easier methods; OSDLPME concentrated multiples higher, lower detection limit; the two methods of traditional Chinese medicine samples free anthraquinone compounds assay results was no significant difference. The second part of the organic solvent and the ionic liquid dispersed liquid microextraction high-performance liquid chromatography analysis of emodin and its metabolites article DLLME (OS-DLLME) of organic solvents and ionic liquids dispersed liquid phase microextraction (IL-DLLME) high performance liquid chromatography for emodin and its metabolites (Aloe emodin, anthraquinone-2 - carboxylic acid, rhein, Dan anthraquinone chrysophanol and emodin) analysis in-depth comparison. Dispersed liquid phase microextraction recovery factors impact on the type of extractant, kind of the dispersing agent, extraction dose, dose dispersed, the pH, ionic strength, and extraction time, centrifugation speed, centrifugation time is optimized. Optimized experimental conditions, the enrichment factor of the OS-DLLME and IL-DLLME method for emodin and its metabolites were 90-295 and 63-192; detection limits were 70 to 400 pg / ml and 100 ~ 600pg / ml; the OS-DLLME's, intra-day and inter-day precision relative standard deviation less than 7.2% and 8.7%, the IL-DLLME's, intra-day and inter-day precision relative standard deviation is less than 5.7% and 6.4%; OS-DLLME 87.1% to 108% of of emodin its metabolites recovery of 87.5% to 106% IL-DLLME on the recoveries of emodin and its metabolites. In comparison, IL-DLLME more convenient, low toxicity and good reproducibility, high enrichment factor of OS-DLLME method sensitivity. For statistical analysis found that the two methods used for analysis of emodin and its metabolites in urine no differences. Aloe emodin, rhein, chrysophanol and emodin emodin metabolites by standard chromatographic retention time control identification; identification by HPLC / MS and found that emodin new metabolites anthraquinone 2 - carboxylic acid and Dan anthraquinone.
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CLC: > Medicine, health > Chinese Medicine > Of Pharmacy > Traditional Chinese medicine chemical
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