倍美力片中的结合雌激素含量测定和GC指纹图谱分析

Studies on the content determination and GC fingerprint of conjugated estrogens from premarin tablets

目的:测定倍美力片中10种结合雌激素成分的含量,建立倍美力片的气相色谱法(GC)指纹图谱,评价倍美力片的内在质量。方法:采用GC法测定倍美力片中10种结合雌激素成分的含量。Rtx-225毛细管柱色谱(15m×0.25mm×0.25μm),柱温为210℃;载气为氢气,流速2.5ml/min,载气分流比为1∶3;载气线速度为60cm/s;以FID为检测器,3-O-甲基雌酮为内标,雌酮为内参照物。结果:通过GC法测定了10批倍美力片中的已知10种成分的含量,确定了10批倍美力片中的20个共有峰,得到分离度和重现性均较好的倍美力片GC指纹图谱;所建立的20个特征峰参数与美国食品药品监督管理局(FDA)提供参数相近。结论:本文所建立的结合雌激素含量测定和GC指纹图谱检测方法准确、可靠,重现性好,可作为结合雌激素产品内在质量控制的标准;倍美力片含有FDA规定的多种成分。

Objective： To determine the contents of ten components from conjugated estrogens （CE） and establish the gas chromatography （GC） fingerprint of premarin tablets for the quality evaluation. Methods： The GC method was used with Rtx -225 column （15 m×0.25 mm×0.25 μm） ; The detector was a flameionization detector（FID） ; The column was held at 210℃ ; The carrier gas was hydrogen flowing at the rate of 2.5 ml/min,The split flow rate is 1 to 3 ml per minute, and linear velocity is 60 cm/s; 3-O-methylestro- ne was used as internal standard and estrone was used as internal reference compound. Results： Ten components of conjugated estrogens in premarin tablets were assayed by GC method; GC fingerprint of premarin tablets was obtained which had good reproducibility; 20 common peaks were established by detecting 10 batches of premarin tablets; The data of fingerprint showed much similarity to the data of FDA. Conclusions： The method by GC for content determination and fingerprint was accurate, reliable and had good reproducibility and applicable to the determination of CE drug substance, material and tablets, which could be used as a standard for controlling the quality of CE products; Premarin tablets contained the components as FDA required.