Compositional analysis and quantification of heparin and heparan sulfate by electrospray ionization ion trap mass spectrometry
Compositional analysis and quantification of heparin and heparan sulfate by electrospray ionization ion trap mass spectrometry
复制标题
DOI：
10.1021/ac0340455
复制
发表时间：
2003-07-01
影响因子：
7.4
通讯作者：
Leary, JA
中科院分区：
文献类型：
--
作者：
Saad, OM;Leary, JA
建立了电喷雾电离质谱（ESI-MS）和串联质谱（MSn）联用的新方法，用于硫酸乙酰肝素（HS）和肝素衍生的δ-二糖的定性和定量分析。肝素/HS的非异构体二糖成分的组成分析是从全扫描MS 1光谱使用内标和计算的响应因子为每个二糖。诊断产品离子的异构二糖的MSn光谱用于定量分析的相对量的混合物中的每一种异构体。使用几种质控样品对该方案进行了验证，并显示出令人满意的准确度和精密度。该分析快速、准确，并且在通过MS分析之前不使用纯化或分离步骤，从而减少了传统方法的样品消耗和分析时间。使用这种定量分析程序，从猪和牛的肠粘膜肝素和硫酸乙酰肝素从牛肾的二糖组成的百分比进行了测定。
A new method using a combination of electrospray ionization mass spectrometry (ESI-MS) and tandem mass spectrometry (MSn) was developed for the identification and quantitative analysis of eight heparan sulfate (HS)and heparin-derived Delta-disaccharides obtained by enzymatic depolymerization. The compositional analysis of nonisomeric disaccharide constituents of heparin/HS was achieved from full-scan MS1 spectra using an internal standard and a calculated response factor for each disaccharide. Diagnostic product ions from MSn spectra of isomeric disaccharides were used for the quantitative analysis of the relative amounts of each of the isomers in mixtures. The protocol was validated using several quality control samples and showed satisfactory accuracy and precision. The analysis is rapid, accurate, and uses no purification or separation steps prior to analysis by MS, thus reducing sample consumption and analysis time of traditional methods. Using this quantitative analysis procedure, percentages of disaccharide compositions for heparins from porcine and bovine intestinal mucosa and heparan sulfate from bovine kidney were determined.