Gas chromatography—mass spectrometry of some prostanoids with new derivatizing agents : Application to the analysis of 13,14-dihydro-15-ketoprostaglandin F2α
Gas chromatography—mass spectrometry of some prostanoids with new derivatizing agents : Application to the analysis of 13,14-dihydro-15-ketoprostaglandin F2α
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使用新型衍生剂对某些前列腺素进行气相色谱-质谱分析：在 13,14-二氢-15-酮前列腺素 F2α 分析中的应用
DOI：
10.1016/s0021-9673(00)96124-7
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发表时间：
1987
影响因子：
4.1
通讯作者：
Shozo Yamamoto
中科院分区：
文献类型：
--
作者：
K. Yamashita;Keiko Watanabe;M. Ishibashi;H. Miyazaki;K. Yokota;K. Horie;Shozo Yamamoto
13，14-二氢-15-酮基前列腺素（PG）F2α与PGD 2、PGE 2和PGF 2 α在10-15 min内完全分离，转化为甲酯-正丁基肟-二甲基异丙基硅醚（ME-nBO-DMiPS）或ME-nBO-环二乙基硅烯（DES）衍生物。质谱分别通过其固有离子[M - 43]+atm/z596（对于ME-nBO-DMiPS醚）和[M - 73]+atm/z450（对于ME-nBO-DES衍生物）来表征。在高质量区出现相对高强度的特征离子，并将其用于高分辨率模式（M/ΔM= 3500）的选择离子监测，可提高生物体液中13，14-dihydro-15-keto-PGF 2 α检测的选择性。在atm/z450.30下测定[M - 73]+离子时，ME-nBO-DES衍生物13，14-dihydro-15-keto-PGF 2 α的检出限为2 pg，信噪比为4：1。
13,14-Dihydro-15-ketoprostaglandin (PG) F2αwas separated completely from PGD2, PGE2and PGF2α, within 10–15 min by gas chromatography—selected-ion monitoring on a capillary column after conversion to their methyl ester—n-butyloxime—dimethylisopropylsilyl (ME—nBO—DMiPS) ether or ME—nBO—cyclic diethylsilylene (DES) derivatives. The mass spectra were characterized by their inherent ions of [M — 43]+atm/z596 for the ME—nBO—DMiPS ether and of [M — 73]+atm/z450 for the ME—nBO—DES derivatives, respectively. The appearance of the characteristic ions in the high-mass region with relatively high intensity and the use of these ions in selected-ion monitoring in a high-resolution mode (M/ΔM= 3500) made it possible to enhance the selectivity in the detection of 13,14-dihydro-15-keto-PGF2αin biological fluids. The detection limit of the ME—nBO—DES derivative of 13,14-dihydro-15-keto-PGF2αwas found to be 2 pg with a signal-to-noise ratio of 4:1 when the ion of [M — 73]+was monitored atm/z450.30.