复方左炔诺孕酮片和滴丸含量及含量均匀度测定

Determination of assay and content uniformity of compound levonorgestrel tablets and its pills

目的:建立复方左炔诺孕酮片和复方左炔诺孕酮滴丸中炔雌醇和左炔诺孕酮含量测定的高效液相色谱法,考察复方左炔诺孕酮片及滴丸的含量均匀度。方法:采用Waters Symmetry300TM C18色谱柱(4.6mm×150mm,5μm),以乙腈-水(40∶60)为流动相,流速1.0mL·min-1,检测波长为220nm。结果:炔雌醇及左炔诺孕酮的线性范围分别为1.554～31.08μg.mL-1(r=0.9999)和7.549～151.0μg·mL-1(r=0.9999);复方左炔诺孕酮片中炔雌醇和左炔诺孕酮平均回收率(n=3)分别为99.6%～101.8%(RSD为0.55%～1.2%)和99.5%～100.7%(RSD为0.46%～1.6%);复方左炔诺孕酮滴丸中炔雌醇平均回收率(n=3)分别为100.6%～101.1%(RSD为0.92%～1.8%)和97.9%～98.7%(RSD为1.1%～1.9%)。样品检测结果显示,复方左炔诺孕酮滴丸含量均匀度良好,但部分复方左炔诺孕酮片的含量均匀度尚不符合2005年版中国药典的相关规定。结论:建立的HPLC法具有专属性强、灵敏度高、操作简便等特点,并可考察炔雌醇和左炔诺孕酮的含量均匀度,达到严格控制药品质量的目的。

Objective： To establish an HPLC method for determination of assay of ethinylestradiol and levonorgestrel in compound levonorgestrel tablets and its pills, as well as to investigate their content uniformity. Methods： Using Waters Symmetry 300TM C18 column（4.6 mm x 150 mm ,5 I.Lm） ,the mobile phase was acetonitrile -water（40： 60） at a flow rate of 1.0 mL ~ min - ~ and detection wavelength was 220 nm. Results： The linear ranges of ethinylestradi- ol and levonorgestrel were 1. 554 -31.08 μg·mL-1 （r =0. 9999） and 7. 549 - 151.0μg·mL-1 respectively（r = 0. 9999 ）. The average recoveries （ n = 3 ） of ethinylestradiol and levonorgestrel of compound levonorgestrel tablets were 99.6% - 101.8% with RSD of 0.55% - 1.2% and 99.5% - 100.7% with RSD of 0.46% - 1.6% ;The average recoveries（ n = 3 ） of ethinylestradiol and levonorgestrel of compound levonorgestrel pills were 100.6% - 101.1% with RSD of 0.92% -1.8% and 97.9% -98.7% with RSD of 1.1% -1.9%. The content uniformities of compound levonorgestrel pills were good, but some of compound levonorgestrel tablets were not complied with the standard of Chinese Pharmacopoeia 2005 edition. Conclusion：The HPLC method is good in the aspect of selectivity and sensitivity, the HPLC method can be applicable for the determination of assay and content uniformity of com- pound levonorgestrel tablets and its pills. In order to safe and effectively use estrogen contraceptive, we have to con- trol the quality of contraceptive in common used in China.