Automated qualitative and quantitative metabolic profiling analysis of urinary steroids by a gas chromatography-mass spectrometry-data system.
Automated qualitative and quantitative metabolic profiling analysis of urinary steroids by a gas chromatography-mass spectrometry-data system.
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通过气相色谱-质谱数据系统对尿类固醇进行自动定性和定量代谢分析。
DOI：
10.1016/s0021-9673(00)81987-1
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发表时间：
1982
期刊：
影响因子：
--
通讯作者：
Sweeley,CC
中科院分区：
文献类型：
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作者：
Vrbanac,JJ;BraseltonJr,WE;Holland,JF;Sweeley,CC
利用亚甲基保留指数对从气相色谱-质谱仪数据中选择的离子色谱图进行离线反向文库搜索分析的计算机系统(MSSMET)已被应用于尿中类固醇的定性和定量测定。采用熔融石英毛细管色谱柱对几种已发表的尿中类固醇化合物的分离和衍生化方法进行了重现性评价。采用重复性最好的方法，采用填充柱(3-m 3%OV-101)和毛细管柱(50-m OV-101WCOT熔融硅胶)对尿类固醇的MSSMET分析进行评价。使用填充柱可以准确地定量大多数尿类固醇。然而，具有相似的质谱图和在填充柱上的保留行为的尿样类固醇(即雄酮和黄体酮，或3α，11β，17α，21-四羟基-5-β-孕烷-20-酮和DNA)可以用毛细管柱完全分离，并且可以用2秒的扫描周期时间(峰上的10-15个数据点)重复性定量，但不能用更长的扫描周期时间。超载是熔融石英毛细管柱遇到的主要问题。
A computer system (MSSMET), using methylene unit retention indices for an off-line reverse library search analysis of selected ion chromatograms from gas chromatography-mass spectrometry data, has been applied to the qualitative and quantitative determination of urinary steroids. Several published methods for the isolation and derivatization of urinary steroids were evaluated for reproducibility using fused silica capillary column gas chromatography. Using a procedure that gave the greatest reproducibility, MSSMET analyses of urinary steroids were evaluated with packed (3-m 3% OV-101) and capillary (50-m OV-101 WCOT fused silica) columns. Most urinary steroids could be accurately quantitated using the packed column. However, urinary steroids with similar mass spectra and retention behavior on a packed column (i.e., androsterone and etiocholanolone, or 3α,11β,17α,21-tetrahydroxy-5β-pregnane-20-one and 3α,11β,17α,21-tetrahydroxy-5α-pregnane-20-one) were completely separated using the capillary column and could be reproducibly quantitated with a 2-sec scan cycle time (10–15 data points across a peak) but not with a longer scan cycle time. Overloading was the major problem encountered with the fused silica capillary column.