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Bis[6-oxygen-(3-m- Nitrobenzene Sulfonyl-amber Acid-1,4 Uniester-4)]-β-cyclodextrin Was Synthesized And Applied To Stationary Phase Of HPLC And Photometric Analysis

Posted on:2008-10-17Degree:MasterType:Thesis
Country:ChinaCandidate:X YangFull Text:PDF
GTID:2121360242456113Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
This paper outlined the effect of enantiomeric separation in chiral compounds and effect of chiral separation withβ-cyclodextrin andβ-cyclodextrin derivatives. It introduced the application ofβ-cyclodextrin andβ-cyclodextrin derivatives in stationary phase of HPLC and photometric analysis. Bis [6-oxygen-(3-m- nitrobenzene sulfonyl-amber acid-1, 4 uniester-4)]-β-CD (abbr.β-CD-M2) was synthesized and the reaction conditions were optimized. The synthesizedβ-CD-M2 was separated and purified and the goal derivative was confirmed by characterization with Fourier transform infrared spectra, ultraviolet map scanning, NMR, elemental analysis and XRD which had not seen on literature report.The stationary phase of HPLC was synthesized byβ-CD-M2 with silica gel. Two kinds of stationary phase in liquid chromatogram were constructed, which includes the coating type and bonded phase with theβ-CD-M2.The columns were prepared using equipments in our laboratory and enantiomeric of aromatic alcohol was separated. The results showed thatα–benzene ethanol, benzene propanol and mandelic acid could be separated successfully under the selected condition and the mechanism was also analyzed. By comparing the bonded phase with the coating type phase, the restricting of solvent and temperature in the bonded phase was relatively[0] light because it was linked to silica by chemical bond. The experiments could be carried out under either the normal phase or the reverse phase [0]and the peak shape of chromatogram is also symmetrical. The effect of theoretical plates of the column was not reducing after 8 months.The ascorbic acid (abbr. AA) could be detected in beverage by a mimic ascorbic acid dehydrogenase with theβ-CD-M2. The reaction conditions were optimized. The optimum dosage of NAD was 0.2027 g.L-1 and the optimum buffer solution was glycine-sodium hydroxide buffer solution pH10.50. In addition, the optimum ratio of mole between the AA and the mimic enzyme was 27:1. Under optimum conditions, a good liner correlation of the AA was 2.95μg.mL-1—26.50μg.mL-1 and the correlation equation was y=0.107+0.00345x(r=0.998) and the detection limit was 1.00μg.mL-1. The concentration of AA in the beverage sample was 0.38mg.mL-1 which was within range of the Maidong beverage label (0.25 mg.mL-1~0.50 mg.mL-1).
Keywords/Search Tags:Bis[6-oxygen-(3-m-nitrobenzene sulfonyl-amber acid-1,4 uniester-4)]-β-CD, synthesize, HPLC stationary phase, mimic enzyme, photometric analysis
PDF Full Text Request
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