Determination of selenosugars in crude human urine using high-performance liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry.

Determination of selenosugars in crude human urine using high-performance liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry.
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使用高效液相色谱/大气压化学电离串联质谱法测定人粗尿中的硒糖。

DOI:
10.1002/rcm.2843
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发表时间:
2007
期刊:
Rapid communications in mass spectrometry : RCM
影响因子:
--
通讯作者:
S. Pergantis
S. Pergantis
中科院分区:
--
文献类型:
--
作者:
S. Letsiou;V. Nischwitz;P. Traar;K. Francesconi;S. Pergantis

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硒的必需性和毒性之间的差距很小,需要对硒的代谢进行详细的研究,以找到合适的人体硒状况指标。目前的方法定量硒形态在人尿中的分离是基于高效液相色谱法(HPLC)耦合在线元素质谱法(MS),和分子质谱检测技术的潜力,可靠的鉴定和定量硒糖在粗人尿中尚未被利用。现在,我们报告了一种高效液相色谱串联质谱(MS/MS)方法的开发,用于可靠地测定粗人尿液中三种重要的硒尿代谢物,统称为硒糖,即甲基2-乙酰氨基-2-脱氧-1-硒-β-D-半乳糖苷(SeGalNAc)、甲基2-乙酰氨基-2-脱氧-1-硒代-β-D-吡喃葡萄糖苷(SeGluNAc)和甲基2-氨基-2-脱氧-1-硒代-β-D-吡喃半乳糖苷(SeGalNH 2)。反相高效液相色谱法,有和没有阳离子交换保护柱,应用于硒糖的分离,大气压化学电离(APCI)和选择反应监测(SRM)用于选择性和灵敏的检测。硒糖的碰撞诱导解离行为进行了详细研究,使用APCI三重四极杆MS/MS和电喷雾离子阱MS。所开发的方法被施加到尿液样品收集前和后硒补充定量SeGalNAc使用外部校准和标准加入的方法。此外,硒补充后的尿液样品中检测到SeGalNH 2。最后,中性丢失扫描作为一种可能的方法检测未知的甲基硒糖进行了探索。
The narrow gap between essentiality and toxicity of selenium requires detailed investigations on selenium metabolism in order to find suitable indicators for the selenium status in the human body. Current methods for quantitative selenium speciation in human urine are based on separation by high-performance liquid chromatography (HPLC) coupled online with elemental mass spectrometry (MS), and the potential of molecular MS detection techniques for the reliable identification and quantification of selenosugars in crude human urine has not been utilized. Now we report the development of an HPLC tandem mass spectrometric (MS/MS) method for the reliable determination in crude human urine of three significant selenium urinary metabolites, collectively termed selenosugars, namely methyl 2-acetamido-2-deoxy-1-seleno-beta-D-galactopyranoside (SeGalNAc), methyl 2-acetamido-2-deoxy-1-seleno-beta-D-glucopyranoside (SeGluNAc) and methyl 2-amino-2-deoxy-1-seleno-beta-D-galactopyranoside (SeGalNH2). Reversed-phase HPLC, with and without cation-exchange guard columns, was applied for the separation of the selenosugars, and atmospheric pressure chemical ionization (APCI) and selected reaction monitoring (SRM) were used for selective and sensitive detection. The collision-induced dissociation behaviour of the selenosugars was studied in detail using APCI triple quadrupole MS/MS and electrospray ion trap MS. The developed method was applied to urine samples collected prior to and after selenium supplementation for the quantification of SeGalNAc using both external calibration and the method of standard additions. Additionally, SeGalNH2 was detected in urine samples after Se supplementation. Finally, neutral loss scanning was explored as a possible method for the detection of unknown methyl-selenosugars.
DOI: 10.1248/jhs.51.107
发表时间: 2005-04
影响因子: --
作者:
Kazuo T. Suzuki
通讯作者: Kazuo T. Suzuki
液相色谱-电喷雾电离串联质谱法,用于对食用富硒和富硒食品后人尿液中主要硒代谢物进行在线表征、监测和同位素分析。
DOI: --
发表时间: 2005
期刊: Anal.Chim.Acta 555
影响因子: --
作者:
Okajima H;et. al.;植竹勝治;藤井 聡之;佐々木千鶴;S.M.A.Zobayed;E.Dumont
通讯作者: E.Dumont