Roman R, Yates C H, Millar J F, O'Neill J, Zweig J S
J Pharm Sci. 1979 Jun;68(6):733-6. doi: 10.1002/jps.2600680621.
A method was developed for the analysis of testosterone 17-enanthate 3-benzilic acid hydrazone, 17-beta-estradiol 3,17-dienanthate, and estradiol benzoate combinations dissolved in an oily vehicle. Testosterone 17-enanthate 3-benzilic acid hydrazone was separated from the other drugs and vehicle components by chromatography on an acetonitrile-infusorial earth column followed by quantitation using UV spectroscopy. The estradiol esters were separated from the oil by an additional chromatographic step using a heptane-silanized infusorial earth column prior to quantitation by GLC. Subjecting formulations to elevated temperatures resulted in detectable losses for testosterone 17-enanthate 3-benzilic acid hydrazone and 17-beta-estradiol 3,17-dienanthate. For both drugs, degradation was due to hydroxysis; the degradation products, testosterone 17-enanthate and 17-beta-estradiol 17-enanthate, did not interfere with the intact drug determination. Methods also were developed to estimate degradation product levels in the formulation.
已开发出一种用于分析溶解在油性赋形剂中的庚酸睾酮3-二苯乙醇酸腙、17β-雌二醇3,17-二庚酸酯和苯甲酸雌二醇组合物的方法。庚酸睾酮3-二苯乙醇酸腙通过在乙腈-硅藻土柱上进行色谱分离，与其他药物和赋形剂成分分离，然后使用紫外光谱法进行定量。在通过气相色谱法定量之前，雌二醇酯通过使用庚烷-硅烷化硅藻土柱的额外色谱步骤与油分离。将制剂置于高温下会导致庚酸睾酮3-二苯乙醇酸腙和17β-雌二醇3,17-二庚酸酯出现可检测到的损失。对于这两种药物，降解是由于水解；降解产物庚酸睾酮和17β-雌二醇17-庚酸酯不干扰完整药物的测定。还开发了估计制剂中降解产物水平的方法。
