Multidimensional Separations of Intact Phase II Steroid Metabolites Utilizing LC-Ion Mobility-HRMS.
Multidimensional Separations of Intact Phase II Steroid Metabolites Utilizing LC-Ion Mobility-HRMS.
复制标题
利用LC-离子迁移率-HRMS多维分离完整的II相类固醇代谢物。
DOI：
10.1021/acs.analchem.1c02163
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发表时间：
2021-08-10
影响因子：
7.4
通讯作者：
McLean, John A.
中科院分区：
文献类型：
--
作者：
Davis, Don E., Jr.;Leaptrot, Katrina L.;Koomen, David C.;May, Jody C.;Cavalcanti, Gustavo de A.;Padilha, Monica C.;Pereira, Henrique M. G.;McLean, John A.
蛋白同化-雄激素类固醇代谢物的检测和明确鉴定在临床、法医和反兴奋剂分析中至关重要。最近，硫酸盐相II类固醇代谢物在类固醇代谢和药物测试中受到越来越多的关注。在很大程度上，这是因为第二阶段类固醇代谢物排泄时间延长，使其成为跟踪体育运动中类固醇滥用的潜在长期化学标记物。液相色谱-串联质谱（LC-MS/MS）等综合分析方法已用于检测和鉴定人尿液中的葡萄糖醛酸苷和硫酸酯类固醇，具有高灵敏度和可靠性。然而，LC-MS/MS鉴定策略可能受到以下事实的阻碍：II相类固醇代谢物在不同的代谢物标记物中产生非选择性离子片段，限制了依赖于精确质量测量和MS/MS信息的代谢物鉴定的置信度。此外，液相色谱-高分辨率质谱法（LC-MS/MS（HRMS））有时不足以从样品基质（通常为尿液）化学噪声中完全分辨分析物峰，从而进一步使准确鉴定工作复杂化。因此，我们开发了一种液相色谱-离子迁移率-质谱（LC-IM-MS）方法，以增加峰容量，并利用IM衍生的碰撞截面（CCS）值作为额外的分子描述符，以增加选择性，并提高在低浓度下完整类固醇分析的识别。
The detection and unambiguous identification of anabolic-androgenic steroid metabolites are essential in clinical, forensic, and anti-doping analyses. Recently, sulfate phase II steroid metabolites have received increased attention in steroid metabolism and drug testing. In large part, this is because phase II steroid metabolites are excreted for an extended time, making them a potential long-term chemical marker of choice for tracking steroid misuse in sports. Comprehensive analytical methods, such as liquid chromatography-tandem mass spectrometry (LC-MS/MS), have been used to detect and identify glucuronide and sulfate steroids in human urine with high sensitivity and reliability. However, LC-MS/MS identification strategies can be hindered by the fact that phase II steroid metabolites generate non-selective ion fragments across the different metabolite markers, limiting the confidence in metabolite identifications that rely on exact mass measurement and MS/MS information. Additionally, liquid chromatography-high resolution mass spectrometry (LC-MS/MS (HRMS)) is sometimes insufficient at fully resolving the analyte peaks from the sample matrix (commonly urine) chemical noise, further complicating accurate identification efforts. Therefore, we developed a liquid chromatography-ion mobility-mass spectrometry (LC-IM-MS) method to increase the peak capacity and utilize the IM-derived collision cross section (CCS) values as an additional molecular descriptor for increased selectivity and improve identifications of intact steroid analyses at low concentrations.
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影响因子：
2.9
作者：
Balcells, Georgina;Matabosch, Xavier;Ventura, Rosa
通讯作者：
Ventura, Rosa
DOI：
10.1007/s13361-019-02288-2
发表时间：
2019-11-01
影响因子：
3.2
作者：
Dodds, James N.;Baker, Erin S.
通讯作者：
Baker, Erin S.
影响因子：
5.1
作者：
Goodwin CR;Fenn LS;Derewacz DK;Bachmann BO;McLean JA
通讯作者：
McLean JA
影响因子：
2
作者：
Giles, Kevin;Williams, Jonathan P.;Campuzano, Iain
通讯作者：
Campuzano, Iain
影响因子：
7.4
作者：
Bijlsma, Lubertus;Berntssen, Marc H. G.;Merel, Sylvain
通讯作者：
Merel, Sylvain