Analytical method for keratan sulfates by high-performance liquid chromatography/turbo-ionspray tandem mass spectrometry

被引：38

作者：

Oguma, T ^{[1
]}

Toyoda, H ^{[1
]}

Toida, T ^{[1
]}

Imanari, T ^{[1
]}

机构：

[1] Chiba Univ, Fac Pharmaceut Sci, Inage Ku, Chiba 2638522, Japan

来源：

ANALYTICAL BIOCHEMISTRY | 2001年 / 290卷 / 01期

关键词：

keratan sulfates; mass spectrometry; glycosaminoglycans;

D O I：

10.1006/abio.2000.4940

中图分类号：

Q5 [生物化学];

学科分类号：

071010 ; 081704 ;

摘要：

We established a highly sensitive LC/MS/MS method for the analysis of the disaccharides produced from keratan sulfates (KS), It was revealed that the disaccharides produced by keratanase II enzymatic digestion of RS could be determined with high sensitivity by the negative-ion mode of multiple reaction monitoring. Furthermore,monosulfatedanddisulfateddisaccharides can be separated using a short column of Capcell Pak NH2 UG80 (35 mm x 2 mm i.d.). The complete analysis of one sample can be performed within 5 min. The assay method was validated and showed satisfactory sensitivity, precision, and accuracy, which enabled quantitation at subpicomole levels. From the results of analyses of KS obtained from cornea, nasal cartilage, and brain, it was found that the degree of sulfation at the C-6 position of the galactose residues differed among those samples in the following order: nasal cartilage > cornea > brain. Our analytical method is very useful for the analyses of KS in various biological materials and for comparison of the degree of sulfation of KS from various biological samples. (C) 2001 Academic Press.

引用

页码：68 / 73

页数：6

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