Vrbanac J J, Braselton W E, Holland J F, Sweeley C C
J Chromatogr. 1982 Apr 30;239:265-76. doi: 10.1016/s0021-9673(00)81987-1.
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 3 alpha, 11 beta, 17 alpha, 21-tetrahydroxy-5 beta-pregnane-20-one and 3 alpha, 11 beta, 17 alpha, 21-tetrahydroxy-5 alpha-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.
一种计算机系统（MSSMET），利用亚甲基单元保留指数对气相色谱 - 质谱数据中选定离子色谱图进行离线反向库搜索分析，已应用于尿甾体的定性和定量测定。使用熔融石英毛细管柱气相色谱法对几种已发表的尿甾体分离和衍生化方法的重现性进行了评估。采用重现性最佳的方法，用填充柱（3米3% OV - 101）和毛细管柱（50米OV - 101 WCOT熔融石英）对尿甾体进行MSSMET分析。大多数尿甾体使用填充柱可准确定量。然而，在填充柱上具有相似质谱和保留行为的尿甾体（即雄甾酮和表雄甾酮，或3α，11β，17α，21 - 四羟基 - 5β - 孕烷 - 20 - 酮和3α，11β，17α，21 - 四羟基 - 5α - 孕烷 - 20 - 酮），使用毛细管柱可完全分离，并且在2秒扫描周期时间（一个峰上有10 - 15个数据点）下可重现定量，但扫描周期时间较长时则不行。过载是熔融石英毛细管柱遇到的主要问题。
