Selective detection of carbon-13, nitrogen-15, and deuterium labeled metabolites by capillary gas chromatography-chemical reaction interface/mass spectrometry.
Selective detection of carbon-13, nitrogen-15, and deuterium labeled metabolites by capillary gas chromatography-chemical reaction interface/mass spectrometry.
复制标题
通过毛细管气相色谱-化学反应界面/质谱法选择性检测碳 13、氮 15 和氘标记的代谢物。
作者：
D. Chace;F. Abramson
我们已经应用了一种新的化学反应界面/质谱技术（CRIMS）的选择性检测13 C-，15 N-，和2 H-标记苯妥英及其代谢物在尿液中的毛细管气相色谱分离。微波驱动的化学反应界面将材料从其原始形式转化为小分子，其质谱用于识别和量化构成每个分析物的核素。每种元素的存在之后，监测由化学反应界面产生的CO2、NO或H2的同位素变体。通过从观察到的M + 1信号中减去天然存在的同位素的丰度，产生仅显示富集的13 C和15 N的色谱图。通过在m/z 3.0219处测量HD获得2 H（D）的选择性色谱图，分辨率为2000。在色谱图中可鉴别出占总标记化合物不到1.5%的代谢物。在信噪比为2时，测定了尿液中15 N标记代谢物的检测限为380 pg/mL，13 C标记代谢物的检测限为7 ng/mL，氘标记代谢物的检测限为16 ng/mL。根据检查的同位素，使用CRIMS观察到250-1000的线性动态范围。为了鉴别这些标记峰（代谢物），在关闭化学反应界面的情况下重复色谱分析，并在CRIMS实验中发现的保留时间处获得质谱。CRIMS是一种新的分析方法，似乎特别适用于代谢研究。
We have applied a new chemical reaction interface/mass spectrometer technique (CRIMS) to the selective detection of 13C-, 15N-, and 2H-labeled phenytoin and its metabolites in urine following separation by capillary gas chromatography. The microwave-powered chemical reaction interface converts materials from their original forms into small molecules whose mass spectra serve to identify and quantify the nuclides that make up each analyte. The presence of each element is followed by monitoring the isotopic variants of CO2, NO, or H2 that are produced by the chemical reaction interface. Chromatograms showing only enriched 13C and 15N were produced by subtracting the abundance of naturally occurring isotopes from the observed M + 1 signal. A selective chromatogram of 2H (D) was obtained by measuring HD at m/z 3.0219 with a resolution of 2000. Metabolites representing less than 1.5% of the total labeled compounds could be identified in the chromatogram. Detection limits from urine of 380 pg/mL of a 15N-labeled metabolite, 7 ng/mL of a 13C-labeled metabolite, and 16 ng/mL of a deuterium labeled metabolite were determined at a signal to noise ratio of 2. Depending on the isotope examined, a linear dynamic range of 250-1000 was observed using CRIMS. To identify many of these labeled peaks (metabolites), the chromatographic analysis was repeated with the chemical reaction interface turned off and mass spectra obtained at the retention times found in the CRIMS experiment. CRIMS is a new analytical method that appears to be particularly useful for metabolism studies.
稳定同位素在药理学研究中的应用。
影响因子：
21.1
作者：
Baillie,TA
通讯作者：
Baillie,TA
同位素比 (IR) 质谱法在药物代谢研究中的评价。
DOI：
10.1002/bms.1200120911
发表时间：
1985
期刊：
Biomedical mass spectrometry
影响因子：
--
作者：
Nakagawa,A;Kitagawa,A;Asami,M;Nakamura,K;Schoeller,DA;Slater,R;Minagawa,M;Kaplan,IR
通讯作者：
Kaplan,IR