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Application Of Ultra-High Performance Liquid Chromatugraphy-Electrospray Ionization Tandem Mass Spectrometry (UPLC-MS/MS) In Analysis Of Chinese Traditional Medicines And Cosmetics

Posted on:2011-08-15Degree:MasterType:Thesis
Country:ChinaCandidate:K J ZhaoFull Text:PDF
GTID:2144360305484960Subject:Chemistry
Abstract/Summary:PDF Full Text Request
Liquid chromatography-mass spectrometry technology lies in its high sensitivity and selectivity, increasingly widespread, both in the structural characterization of natural products, or cosmetic quality control, can be effectively applied. In this paper, liquid chromatography-mass spectrometry to do the following two studies:1. Extraction and determination of bioactive compounds in Acanthopanax senticosus (AS)Simultaneous extract flavonoids and saponins in AS by ultrasonic assisted extraction, extraction efficiency was measured by ultraviolet-visible spectrophotometry (UV-Vis), investigate the extraction solvent, liquid ratio, extraction time and ultrasonic power four single-factors on the extraction efficiency, and designed L9(34) orthogonal table, selected the optimum extraction conditions:the concentration of ethanol was 70%, the ratio of solid to solution was 1:50, the ultrasonic time was 60min and the ultrasonic power was 90Hz. For the bioactive compounds in crude extracts of AS, of which fragmentation mechanism and chemical structure were studied by UPLC-MS/MS. Most of the active compounds can be detected, of which flavonoids such as quercetin, quercitrin, hyperin, rutin, saponins such as eleutheroside D/E, C, B, B1 and A, and organic acids such as chlorogenic acid, iso chlorogenic acid, isofraxidin, oleanolic acid/ursolic acid, were able to determined and detected by UPLC-MS/MS MRM.2. Analysis and testing methods of restricted and prohibited compounds in hair dyesThe chemical compounds, which can be able to enter the human body during dyeing, are widely used in the hair dye, so there will lead to various diseases with long-term exposure. In this paper, establish the analysis and testing methods of restricted and prohibited compounds, including dye intermediate phenolics and dyes, in hair dye were studied. Using ultrasonic assisted extraction for the sample pretreatment, established the qualitative and quantitative methods of 3 systems (phenols, dyes, phenols and dye) in hair dyes by UPLC/UPLC-MS/MS. (1)7 phenols were separated on a Waters BEH C18 column, the multi-reaction monitoring (MRM) scan mode was employed for the determination. The LOD of the method was below the 0.05μg·mL-1 and the LOQ was below the 0.1μg·mL-1. Average recoveries for the 7 phenols (spiked at the levels of low, medium and high) ranged from 68.80% to 112.50%, with RSD (n=6) between 1.58% and 12.61%; (2) 4 dyes were separated on a Capcell Pak C18 MGⅢcolumn. The LOD was below the 0.01μg·mL-1 and the LOQ was below the 0.05μg·mL-1. Average recoveries for the 4 dyes (spiked at three levels) ranged from 74.60% to 109.15%, with RSD (n=6)< 11.80%; (3) 10 phenols and dyes were separated on a Capcell Pak C18 MGⅢ, the multi-reaction monitoring (MRM) scan mode was employed for the determination, the LOD of the method was between 0.5 and 40μg·L-1, the LOQ was between 1 and 200μg·L-1. Average recoveries for the eight compounds (spiked at three levels) ranged from 61.70%-119.76%, with RSD (n=6)<21.60%.
Keywords/Search Tags:UPLC-MS/MS, Acanthopanax senticosus(AS), Hair dyes
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