[Preparation of 1-(2-naphthyl) -3-methyl-5-pyrazolone as pre-column derivatization reagent for the determination of saccharides using high performance liquid chromatography-mass spectrometry].
Eight saccharides were derivatized using 1-(2-naphthyl)-3-methyl-5-pyrazolone (NMP) as pre-column derivatizing reagent, and separated on a reversed-phase Hypersil ODS 2 column (4.6 mm x 200 mm, 5 microm), by high performance liquid chromatography (HPLC) in conjunction with a gradient elution, detected by a diode array detector (DAD), and identified by electrospray ionization-mass spectrometry (ESI-MS) in positive ion mode. NMP reacted with reductive saccharides easily in the presence of 17% ammonia water at 70 degrees C. All linear correlation coefficients for saccharide derivatives were over 0.998 5. The detection limits (at signal-to-noise of 3:1) were 0.58 - 1.1 pmol for saccharide derivatives. The characteristic fragment ions, especially m/z 473, from the cleavage of NMP-labeled saccharides exhibited high regularity for the identification of the composition of saccharide mixture. The established method is sensitive and repeatable for the determination of saccharides.
Sun
Zhiwei
Z
Key Laboratory of Life-Organic Analysis of Sandong Province, College of Chemistry Science, Qufu Normal University, Qufu 273165, China. sunzhiw@126.com
Liu
Lingjun
L
Hu
Baojun
B
Sheng
Xiao
X
Wang
Xiaoyan
X
Suo
Yourui
Y
You
Jinmao
J
D053000:Analytic Sample Preparation Methods / Q000379:methods*; D002851:Chromatography, High Pressure Liquid / Q000379:methods* / Q000592:standards; D056148:Chromatography, Reverse-Phase; D006863:Hydrogen-Ion Concentration; D007202:Indicators and Reagents / Q000737:chemistry; D057230:Limit of Detection; D016014:Linear Models; D013058:Mass Spectrometry / Q000379:methods* / Q000592:standards; D009281:Naphthalenes / Q000737:chemistry*; D011134:Polysaccharides / Q000032:analysis* / Q000737:chemistry* / Q000302:isolation & purification; D047069:Pyrazolones / Q000737:chemistry*; D012015:Reference Standards; D015203:Reproducibility of Results; D013696:Temperature
C527199:1-(2-naphthyl)-3-methyl-5-pyrazolone; D007202:Indicators and Reagents; D009281:Naphthalenes; D011134:Polysaccharides; D047069:Pyrazolones