Ishibashi M, Nakagawa Y, Harima N, Hishinuma T, Mizugaki M
Research Laboratories, Nippon Kayaku Co., Ltd., Tokyo, Japan.
Biol Mass Spectrom. 1994 Oct;23(10):612-20. doi: 10.1002/bms.1200231003.
Gas chromatography/high-resolution selected ion monitoring (GC/HR-SIM) for the determination of 11-dehydrothromboxane B2 (11-dehydro-TXB2) in human urine is described. Combined use of the lactone ring opening reaction and dimethylisopropylsilylation has been adopted for the analysis of 11-dehydro-TXB2, to give a new chemically stable derivative. The feasibility of using this derivative for the analysis of 11-dehydro-TXB2 in human urine has been evaluated. Following the addition of 18O2-labelled analogue, for use as an internal standard, the samples were extracted using chromatographic separation with Bond Elut C18 and silica gel. Derivatization of the extracted 11-dehydro-TXB2 was followed by GC/SIM at resolution of 5000. This method enables selective detection of 11-dehydro-TXB2 in human urine without serious interference from other endogenous substances. In 11 volunteers, the mean urinary excretions of 11-dehydro-TXB2 was 547.6 +/- 217.6 ng per day.
本文描述了用于测定人尿中11-脱氢血栓素B2（11-dehydro-TXB2）的气相色谱/高分辨率选择离子监测（GC/HR-SIM）方法。采用内酯开环反应和二甲基异丙基硅烷化联用技术分析11-脱氢-TXB2，得到一种新的化学稳定性衍生物。评估了使用该衍生物分析人尿中11-脱氢-TXB2的可行性。加入18O2标记类似物作为内标后，样品采用Bond Elut C18和硅胶进行色谱分离萃取。萃取后的11-脱氢-TXB2进行衍生化处理，然后在分辨率为5000的条件下进行GC/SIM分析。该方法能够选择性检测人尿中的11-脱氢-TXB2，不受其他内源性物质的严重干扰。在11名志愿者中，11-脱氢-TXB2的平均尿排泄量为每天547.6±217.6 ng。
