Watanabe K, Yamashita K, Ishibashi M, Hayashi Y, Yamamoto S, Miyazaki H
Research Laboratories, Pharmaceuticals Group, Nippon Kayaku Co., Tokyo, Japan.
J Chromatogr. 1989 May 12;468:383-94. doi: 10.1016/s0021-9673(00)96333-7.
Simple and effective purification for quantitation of trace amounts of 11-dehydrothromboxane B2 (11-dehydro-TXB2) in human urine by gas chromatography-selected-ion monitoring (GC-SIM) was achieved. The procedure is based on stepwise elution of the methyl ester derivative from a silica gel column with n-hexane-ethyl acetate (1:1) after washing the column with n-hexane-ethyl acetate (2:1). After the methyl ester has been converted into the corresponding dimethylisopropylsilyl ether, GC-SIM is carried out by monitoring the ion at m/z 539.32 for 11-dehydro-TXB2 and that at m/z 543.33 for its 18O2-labelled variant as an internal standard. The detection limit is 2 pg per injection with a signal-to-noise ratio of 5:1. The method was applied to the determination of 11-dehydro-TXB2 in human urine.
通过气相色谱 - 选择离子监测（GC - SIM）实现了对人尿中痕量11 - 脱氢血栓素B2（11 - dehydro - TXB2）进行定量的简单有效纯化。该方法基于在用正己烷 - 乙酸乙酯（2:1）冲洗硅胶柱后，用正己烷 - 乙酸乙酯（1:1）从硅胶柱上逐步洗脱甲酯衍生物。在甲酯转化为相应的二甲基异丙基硅醚后，通过监测m/z 539.32处的离子来测定11 - dehydro - TXB2，监测m/z 543.33处的离子来测定其18O2标记变体作为内标进行GC - SIM。检测限为每次进样2 pg，信噪比为5:1。该方法应用于人尿中11 - dehydro - TXB2的测定。
