Swiss BioQuant AG, Kägenstrasse 18, 4153 Reinach, Switzerland.
J Chromatogr B Analyt Technol Biomed Life Sci. 2012 Jul 15;901:67-71. doi: 10.1016/j.jchromb.2012.05.044. Epub 2012 Jun 16.
An HPLC-MS/MS method was developed and validated for the quantification of 6-keto prostaglandin F1α, the stable hydrolysis product of prostacyclin, and its metabolites 2,3-dinor-6-keto prostaglandin F1α and 6,15-diketo-13,14-dihydro prostaglandin F1α in human plasma. For sample preparation, a solid phase extraction step was combined with a column switching approach for analytes enrichment and further sample clean-up of the processed sample. The assay was validated in the concentration range 50.0-5000 pg/mL for 6-keto prostaglandin F1α and 6,15-diketo-13,14-dihydro prostaglandin F1α, and 100-10,000 pg/mL for 2,3-dinor-6-keto prostaglandin F1α. The inter-batch precision was better than 12.7%, 9.2%, and 9.4% for 6-keto prostaglandin F1α, 2,3-dinor-6-keto prostaglandin F1α, and 6,15-diketo-13,14-dihydro prostaglandin F1α, respectively. The inter-batch accuracy was between 97.3% and 100.8% for 6-keto prostaglandin F1α, between 97.5% and 103.0% for 2,3-dinor-6-keto prostaglandin F1α, and between 92.0% and 100.0% for 6,15-diketo-13,14-dihydro prostaglandin F1α. Further it has been demonstrated that the analytes were stable in plasma for 20 h at room temperature, during three freeze-and-thaw cycles, for 96 days at -25 °C storage temperature, and 50h in the autosampler tray at room temperature.
建立并验证了高效液相色谱-串联质谱法（HPLC-MS/MS），用于检测人血浆中前列环素的稳定水解产物 6-酮前列腺素 F1α及其代谢产物 2,3-二去甲-6-酮前列腺素 F1α和 6,15-二酮-13,14-二氢前列腺素 F1α的含量。在样品制备过程中，采用固相萃取和柱切换技术，实现对分析物的富集和预处理样品的进一步净化。6-酮前列腺素 F1α、6,15-二酮-13,14-二氢前列腺素 F1α和 2,3-二去甲-6-酮前列腺素 F1α的检测浓度范围分别为 50.0-5000 pg/mL、100-10000 pg/mL 和 100-10000 pg/mL。6-酮前列腺素 F1α、2,3-二去甲-6-酮前列腺素 F1α和 6,15-二酮-13,14-二氢前列腺素 F1α的批内精密度均小于 12.7%、9.2%和 9.4%，批间准确度均在 97.3%-100.8%、97.5%-103.0%和 92.0%-100.0%之间。进一步研究表明，在室温下放置 20 h、经过 3 次冻融循环、-25°C 保存 96 天以及在室温下置于自动进样器托盘内 50 h 后，血浆中的分析物均稳定。
