Wickramasinghe A J, Shaw R S
Biochem J. 1974 Jul;141(1):179-87. doi: 10.1042/bj1410179.
A sensitive electron-capture gas-liquid-chromatographic method for the determination of sub-nanogram quantities of prostaglandin F(2alpha) was developed. The method is based on the sub-microgram scale conversion of the prostaglandin into the electron-capturing pentafluorobenzyl ester, and analysis of the latter as the tris-trimethylsilyl ether. The lower limit of detection was 12.5pg of the ester injected ;on-column' as the silylated product. The method was successfully applied to the determination of prostaglandin F(2alpha) in monkey plasma. The specificity of the analytical procedure was increased by incorporating a thin-layer chromatographic fractionation before gas-liquid chromatography. The utility of the analytical methodology developed was demonstrated by its application to the determination of plasma concentrations of intact prostaglandin F(2alpha) in a Rhesus monkey, after subcutaneous administration of a single dose of prostaglandin F(2alpha). The electron-capture gas-liquid-chromatographic assay is compared with the radioimmunoassay and the gas-liquid-chromatographic-mass-spectrometry assay for the determination of prostaglandin F(2alpha).
已开发出一种灵敏的电子捕获气液色谱法,用于测定纳克以下量的前列腺素F(2α)。该方法基于将前列腺素在亚微克量级上转化为电子捕获的五氟苄酯,并将后者作为三 - 三甲基硅醚进行分析。检测下限为进样“柱上”作为硅烷化产物的酯12.5皮克。该方法已成功应用于猴血浆中前列腺素F(2α)的测定。通过在气液色谱之前进行薄层色谱分级分离,提高了分析程序的特异性。通过将其应用于恒河猴皮下单次注射前列腺素F(2α)后血浆中完整前列腺素F(2α)浓度的测定,证明了所开发分析方法的实用性。将电子捕获气液色谱法与放射免疫分析法和气液色谱 - 质谱分析法进行比较,以测定前列腺素F(2α)。