Bishara R H, Rutherford B S, Dinner A
J Pharm Sci. 1975 Jul;64(7):1210-3. doi: 10.1002/jps.2600640719.
A rapid, sensitive, and accurate GLC method of analysis of a new estrogenic drug, 17 alpha-ethynylestriol 3-cyclopentyl ether, was developed. The drug and the internal standard, tetratriacontane, are dissolved in chloroform, and an aliquot is heated with N-trimethylsilylimidazole at 80 degrees for 30 min. The silylated sample is chromatographed using a column packed with 1% methyl vinyl silicone gum on Gas Chrom Q. Quantitation is achieved by computer calculation of the peak area ratios. The observed peak is the 16alpha,17beta-bistrimethylsilyl derivative of the new drug substance. The GLC method was applied to the quantitative determination of the estrogenic compound in a tablet formulation containing 25 mug/tablet.
开发了一种快速、灵敏且准确的气相色谱法，用于分析一种新型雌激素药物17α-乙炔基雌三醇3-环戊基醚。该药物和内标三十四烷溶解于氯仿中，取一份等分试样与N-三甲基硅咪唑在80℃加热30分钟。将硅烷化后的样品用填充有1%甲基乙烯基硅橡胶的气相色谱柱进行色谱分析，在Gas Chrom Q上进行。通过计算机计算峰面积比来进行定量。观察到的峰是新药物的16α,17β-双三甲基硅烷基衍生物。该气相色谱法用于定量测定片剂制剂中含25μg/片的雌激素化合物。
