REVERSED-PHASE LIQUID-CHROMATOGRAPHIC ANALYSIS OF DNS-SUGARS - OPTIMIZATION OF DERIVATIZATION AND CHROMATOGRAPHIC PROCEDURES AND APPLICATIONS TO NATURAL SAMPLES

REVERSED-PHASE LIQUID-CHROMATOGRAPHIC ANALYSIS OF DNS-SUGARS - OPTIMIZATION OF DERIVATIZATION AND CHROMATOGRAPHIC PROCEDURES AND APPLICATIONS TO NATURAL SAMPLES
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DOI:
10.1016/s0021-9673(01)88209-1
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发表时间:
1983-01-01
期刊:
JOURNAL OF CHROMATOGRAPHY
影响因子:
--
通讯作者:
JOHNSON, L
JOHNSON, L
中科院分区:
其他
文献类型:
--
作者:
MOPPER, K;JOHNSON, L

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详细研究了5-二甲氨基萘-1-磺酰肼(dns -肼)作为柱前荧光标记试剂的潜力。反应动力学(以及糖腙的产率)受到几个相互作用参数的强烈影响。然而,当观察到适当的预防措施时,获得了精度很高的定量结果(0.5 nmol水平下SD .apprxeq. +- 0.0.4%)。检出限为2 ~ 5 pmol/注射糖。用dns衍生化法和常规糖分析仪对木材水解物进行了分析,结果非常吻合。采用反相高效液相色谱法,以乙腈-乙酸水溶液(甲酸)为流动相,对14种糖衍生物进行了等压分离。20分钟。与离线技术相比,使用预柱代替注入循环的在线样品清理更加快速和有效。对生理液体[尿液]、饮料[橙汁]和木材水解物的应用进行了说明。
The potential of 5-dimethylaminonaphthalene-1-sulfonylhydrazine (Dns-hydrazine) as a precolumn fluorimetric labeling reagent for reducing sugars was examined in detail. The kinetics of the reaction (and therefore yields of sugar hydrazones) were strongly affected by several interacting parameters. However, when appropriate precautions were observed, quantitative results with excellent precision were obtained (SD .apprxeq. .+-.0.4% at the 0.5 nmol level). The detection limit was 2-5 pmol/injected sugar. Analysis of a wood hydrolysate with the Dns-derivatization method and with a conventional sugar analyzer gave excellent agreement. Using reversed-phase high-performance liquid chromatography and a mobile phase of acetonitrile-aqueous acetic (or formic) acid, 14 sugar derivatives were separated isocratically in .apprx. 20 min. On-line sample clear-up, using a precolumn in place of the injection loop, was more rapid and effective than off-line techniques. Applications to physiological fluids [urine], beverages [orange juice] and wood hydrolysates are illustrated.