Determination of monosaccharide composition of polysaccharides in Polygonum officinale and its adulterants by UPLC-MS/MS
Objective:To establish an ultra-performance liquid chromatography-tandem quadrupole mass spectrometry(UPLC-MS/MS)method for the determination of the monosaccharide composition of polysaccharides from Polygonum multiflorum Thunb.,which can be used to reveal the differences between its raw herb,processing herb,tuber fleeceflower stem(different parts)and mixed forgeries in the market,i.e.,Airpotato Yam Rhizome,Ciliatenerve Knotweed Root,and Bunge Auriculate Root.Methods:The polysaccharides were obtained by hydrolysis using trifluoroacetic acid and the hydrolysis product was derivatized by adding 1-phenyl-3-methyl-5-pyrazolinone(PMP).The separation was carried out on a Waters ACQUITY UPLC BEH C18 analytical column(100 mm x2.1 mm,1.7 µm)with acetonitrile and buffered salt solution(1 mmol·L-1 ammonium acetate-0.175％acetic acid)as the mobile phase using a gradient elution.The separation was carried out at a flow rate of 0.2 mL·min-1.The column temperature was set at 35 ℃ and the injection volume was 2 µL.The determination was carried out in multiple reaction monitoring(MRM)in electrospray positive ionization mode and quantified by internal standard method.Results:The polysaccharide composition of raw herb consisted of 10 monosaccharides:mannose,ribose,rhamnose,glucuronic acid,galacturonic acid,glucose,galactose,arabinose,xylose and fucose,with the content percentages of0.38％,0.08％,0.99％,0.70％,8.56％,84.55％,2.11％,2.45％,0.11％and 0.08％.The monosaccharide composition of the processing herb is the same as that of the raw herb,but differences exist in the monosaccharide content,mainly in glucose and galacturonic acid.The types of monosaccharide composition in tuber fleeceflower stem are different from those of the raw herb.There are also major differences between the three mixes and the raw herb,mainly in the composition of the monosaccharides.The glucose content of the raw herb was higher than that of the three mixes,while the lower level of galactose.Conclusion:A PMP pre-column derivatization-UPLC-MS/MS method was developed for the analysis of the monosaccharide composition of polysaccharides from Polygonum multiflorum Thunb..The method was also used for the identification and analysis of its raw herb and processing herb,tuber fleeceflower stem,and mixed forgeries.The method is of high sensitivity and short analysis time,which can provide a reference for the improvement of its quality control and the differentiation of common mixed forgeries.
Polygonum multiflorum Thunb.polysaccharidemonosaccharide compositionultra performance liquid chromatography-tandem mass spectrometrymixed forgeries
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