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首页> 外文期刊>Journal of mass spectrometry: JMS >Comparison of CID versus ETD-based MS/MS fragmentation for the analysis of doubly derivatized steroids
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Comparison of CID versus ETD-based MS/MS fragmentation for the analysis of doubly derivatized steroids

机译：基于CID与基于ETD的MS / MS片段比较，以分析双衍生类固醇

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Electrospray ionization coupled with collision-induced dissociation (CID) and tandem mass spectrometry (MS/MS) is a commonly used technique to analyze the chemical composition of steroids. However, steroids are structurally similar compounds, making it difficult to interpret their product-ion spectra. Electron transfer dissociation (ETD), a relatively new technique for protein and peptide fragmentation, has been shown to providemore detailed structural information. In this study, we compared the ability of CID with that of ETD to differentiate between eight 3,20-dioxosteroids that had been derivatizated with a quaternary ammoniumsalt, Girard reagent P (GirP), at room temperature or after exposure to microwave irradiation to generate doubly charged ions. We found that the derivatization of steroid with GirP hydrazine occurred in less than 10 min when the reaction was carried out in the presence of microwave irradiation compared to 30min when the reaction was carried out at room temperature. According to the MS/MS spectra, CID provided rich, structurally informative ions; however, the spectra were complex, thereby complicating the peak assignment. In contrast, ETD generated simpler spectra,making it easier to recognize individual peaks. Remarkably, both CID and ETD were allowed to differentiate of steroid isomers, 17α-hydroxyprogesterone (17OHP) and deoxycorticosterone (DOC), but the signature ions obtained from CID were less intense than those generated by ETD, which generated much clearer spectra. These results indicate that ETD in conjunction with CID can provide more structural information for precise characterization of steroids.
机译：电喷雾电离结合碰撞诱导解离（CID）和串联质谱（MS / MS）是分析类固醇化学成分的常用技术。但是，类固醇是结构相似的化合物，因此难以解释其产物离子光谱。电子转移解离（ETD）是一种相对较新的蛋白质和肽片段化技术，已被证明可提供更详细的结构信息。在这项研究中，我们比较了CID和ETD区分在室温下或暴露于微波辐射后用季铵盐，吉拉德试剂P（GirP）衍生化的8种3,20-二氧代类固醇的能力。双电荷离子。我们发现，当在微波辐射存在下进行反应时，用GirP肼进行类固醇的衍生反应少于10分钟，而在室温下进行反应则为30分钟。根据MS / MS光谱，CID提供了丰富的，结构丰富的离子。但是，谱图很复杂，从而使峰分配变得复杂。相比之下，ETD生成的光谱更简单，从而更易于识别各个峰。值得注意的是，CID和ETD都可以区分类固醇异构体17α-羟基孕酮（17OHP）和脱氧皮质酮（DOC），但从CID获得的特征离子强度不如ETD产生的离子强，因此产生的光谱更清晰。这些结果表明ETD与CID结合可以提供更多的结构信息，以精确表征类固醇。

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