HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY OF CARDIAC STEROIDS
HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY OF CARDIAC STEROIDS
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强心类固醇的高效液相色谱-串联质谱法
DOI：
10.1081/jlc-100101801
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发表时间：
1999
影响因子：
1.3
通讯作者：
H. Nakazawa
中科院分区：
文献类型：
--
作者：
T. Higashi;N. Nakayama;K. Shimada;H. Kasai;H. Nakazawa
采用离子陷阱质谱仪的高效液相色谱-串联质谱仪(LS/MSN)对具有代表性的心脏类固醇进行了分析。在具有极性残基(琥珀酸精氨酸)的情况下，正电喷雾电离(ESI)比常压化学电离(APCI)灵敏50倍，并提供了关于苷元和琥珀酸精氨酸的相对分子质量和结构的信息。相应的蟾酥配基对APCI阳性反应的敏感性是ESI的2倍。正APCI型地高辛的质谱图表明，碎片离子不仅来源于苷元，而且还由糖的损失形成。在具有不寻常糖键的心脏糖苷上观察到二恶烷环的裂解。考察了这些化合物的快原子轰击质谱图，并与LC/MSN的数据进行了比较。
High performance liquid chromatography-tandem mass spectrometry (LS/MSn) utilizing an ion trap mass spectrometer has been used for the analyses of representative cardiac steroids. In the case of bufotoxin having a polar residue (suberoylarginine), the positive-electrospray ionization (ESI) was 50 times more sensitive than the atmospheric pressure chemical ionization (APCI) and provided information concerning the molecular weight as well as the structures of both aglycone and suberoylarginine. The corresponding bufogenin showed 2 times better sensitivity in the positive-APCI than ESI. The mass spectrum of digoxin with the positive-APCI showed fragment ions not only derived from aglycone but also formed by losses of sugars. The cleavage of the dioxane ring has been observed on the cardiac glycoside having an unusual sugar linkage. Fast atom bombardment mass spectra of these compounds were examined and compared with the data obtained from LC/MSn.