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[Objective]To establish the quantitative detection method for the monosaccharide composition in the polysaccharides of Juglans sigillata D. shells. [Methods]Using trifluoroacetic acid to hydrolyze the polysaccharides of J. sigillata shells,1-phenyl-3-methyl-5-pyrazolone (PMP) was added into the hydrolysate of polysaccharides for pre-column derivatization. PMP derivative of monosaccharide was analyzed by high performance liquid chromatography (HPLC) . Chromatographic column was Agilent Venusil XBP-C18 (4.6 mm × 250 mm,5 μm) ; mobile phase was acetonitrile solution ammonium acetate buffer (pH 5. 5,19∶ 81,V/V) ; detection wavelength was 250 nm; column temperature was 30 ℃ ; and volume flow was 1 mL/min. [Results] Polysaccharides of J. sigillata shells were composed of 11 monosaccharides,which were D-glucuronic acid,D-mannose,galactose,D-arabinose,rhamnose,D-galacturonic acid,glucose and other 4 monosaccharides not detected. The linear ranges of D-mannose,rhamnose,D-glucuronic acid,D-galacturonic acid,glucose,galactose and D-arabinose were 0. 041 8-2. 09,0. 045 9 2. 295,0. 043 5 2. 175,0. 042 7 2. 135,0. 040 5 2. 026,0. 043 9 2. 195 and 0. 047 5 2. 375 μg/mL,respectively. And their average recovery rates were 95. 9% ,103. 1% ,104. 6% ,97. 5% ,95. 8% ,87. 5% and 98. 1% ,respectively. The RSD values were all smaller than 3. 0% . Among them,D-arabinose had relatively high average content. [Conclusions]This method could accurately detect the monosaccharides and their contents in the polysaccharides of J. sigillata shells.
[Objective] To establish the quantitative detection method for the monosaccharide composition in the polysaccharides of Juglans sigillata D. shells. [Methods] Using trifluoroacetic acid to hydrolyze the polysaccharides of J. sigillata shells, 1-phenyl-3-methyl-5-pyrazolone (PMP) was added into the hydrolysate of polysaccharides for pre-column derivatization. PMP derivative of monosaccharide was analyzed by high performance liquid chromatography (HPLC). Chromatographic column was Agilent Venusil XBP- C18 (4.6 mm × 250 mm, 5 μm) The mobile phase was acetonitrile (pH 5.5, 19:81, V / V); detection wavelength was 250 nm; column temperature was 30 ° C .; and volume flow was 1 mL / min. [Results] Polysaccharides of J The linear ranges of D-mannose, rhamnose , D-glucuronic acid, D. -galacturonic acid, glucose, galactose and D-arabinose were 0. 041 8-2. 09,0. 045 9 2. 295,0. 043 5 2. 175,0. 042 7 2. 135,0. 040 5 2 .,06,0. 043 9 2. 195 and 0. 047 5 2. 375 μg / mL, respectively. And their average recovery rates were 95.9%, 103.1%, 104.6%, 97.5% 95. 8%, 87.5% and 98. 1%, respectively. The RSD values were all smaller than 3.0%. Among them, D-arabinose had relatively high content. [Conclusions] This method could accurately detect the monosaccharides and their contents in the polysaccharides of J. sigillata shells.