Dimethylisopropylsilyl ether derivatives in gas chromatography mass spectrometry of prostaglandins and thromboxane B2
Dimethylisopropylsilyl ether derivatives in gas chromatography mass spectrometry of prostaglandins and thromboxane B2
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二甲基异丙基甲硅烷基醚衍生物气相色谱质谱法测定前列腺素和血栓素 B2
DOI：
10.1002/bms.1200081102
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发表时间：
1981
期刊：
影响因子：
--
通讯作者：
M. Katori
中科院分区：
文献类型：
--
作者：
H. Miyazaki;M. Ishibashi;K. Yamashita;Y. Nishikawa;M. Katori
采用SE-30毛细管柱，在15 min内完全分离了前列腺素F1 α和前列腺素F2 α甲酯的二甲基异丙基硅醚衍生物和前列腺素D2、前列腺素E1、前列腺素E2、6-酮前列腺素F1 α和血栓素B2甲酯。这些衍生物的亚甲基单元值略大于相应的二甲基-正丙基甲硅烷基醚衍生物。二甲基异丙基甲硅烷基醚衍生物的使用使得可以进行未被三甲基甲硅烷基醚衍生物分离的PG和血栓烷B2的基线分离。这些二甲基异丙基甲硅烷基醚衍生物的质谱裂解类似于相应的三甲基甲硅烷基醚衍生物，在以前的论文中报道。它们的质谱由分子离子[M]+表征，离子[M-15]+和[M-43]+与先前报道的羟基类固醇二甲基异丙基甲硅烷基醚衍生物中的离子类似。离子[M-34]+，它是通过从[M]+中消除异丙基而产生的，观察到一个强烈的峰值。该离子在高质量区的出现对于定量生物体液中痕量的PG和血栓烷B2非常有用，而不干扰内源性物质，通过选择离子监测。当监测离子[M-43]+（m/z 625）时，发现PGF 2 α甲酯的二甲基异丙基硅醚衍生物的检测限为5 pg，信噪比为10：1。
The dimethylisopropylsilyl ether derivatives of PGF1α and PGF2αmethyl esters and PGD2, PGE1, PGE2, 6-Keto PGF1α and thromboxane B2 methoxime-methyl esters were separated completely within 15 min by gas chromatography using open tubular glass capillary column coated with SE-30. The methylene unit values of these derivatives were slightly greater than those of the corresponding dimethyl-n-propylsilyl ether derivatives. The use of the dimethylisopropylsilyl ether derivatives made it possible to perform the baseline separation of PGs and thromboxane B2 which were not separated by the trimethylsilyl ether derivatives. The mass spectral fragmentation of these dimethylisopropylsilyl ether derivatives was similar to those of the corresponding trimethysilyl ether derivatives, reported in a previous paper. Their mass spectra were characterized by the molecular ion, [M]+., and the ions [M—15]+ and [M—43]+ like those in the hydroxysteroid dimethylisopropylsilyl ether derivatives reported previously. The ion [M—34]+, which is produced by the elimination of isopropyl group from [M]+., was observed as an intense peak. The appearance of this ion in the high mass region was very useful for quantitation of trace amounts of PGs and thromboxane B2 in biological fluids without disturbance of endogenous substances by selected ion monitoring. The detection limit of the dimethylisopropylsilyl ether derivative of PGF2α methyl ester was found to be 5 pg with a signal-to-noise ratio of 10:1 when monitoring the ion [M—43]+ (m/z 625).