香黄通便胶囊中大黄素、大黄酚含量测定的研究  

Study of content determination of Emodin and Chrysophanold and in Xianghuangtongbian Capsule

作　　者：祁秀玲[1] 孙会昌 王晓琦 付秀英 王立岭 李国岭 

机构地区：[1]沧州医学高等专科学校,河北沧州061000 [2]河北省沧州市食品药品检验所,河北沧州061000

出　　处：《中国医药导报》2014年第17期93-95,99,共4页China Medical Herald

基　　金：河北省科学技术研究与发展计划(第十七批)项目(编号12272507)

摘　　要：目的采用高效液相色谱法，对香黄通便胶囊中大黄素、大黄酚的含量测定进行研究。方法①高效液相色谱法：检测大黄素、大黄酚的含量。参考文献选择合适的固定相，调整流动相组成、配比、流速以及柱温，在最大吸收波长下测定，使指标峰分离完全，理论塔板数符合要求。②线性范围考察：配制系列浓度的对照品溶液，以色谱峰的峰面积为纵坐标，以进样浓度为横坐标，进行线性回归，得回归曲线并考察线性范围。③方法学考察：分别考察测定方法的重复性、中间精密度、重现性、耐用性、稳定性和加样回收率。④样品含量测定：取三批样品分别按上述方法测定指标成分的含量。结果香黄通便胶囊中大黄素、大黄酚色谱条件为：WelchUltimateXB-C18色谱柱，流动相：甲醇-0．1％磷酸（80：20），流速1mL／min，柱温25℃，检测波长254nm。大黄素、大黄酚分别在1．4～70、19．8～990μg／mL范围内线性关系良好，r分别为0．9999、0．9999。该方法下大黄素、大黄酚重复性、中间精密度、重现性、耐用性、在12h内稳定性和加样回收率的RSD分别为：0．58％、0．15％，1．25％、0．32％，1．48％、0．49％，1．35％、0．43％，1．25％、0．13％，0．62％、0．46％。样品中大黄素、大黄酚总含量不低于3.3mg／粒。结论以较为公认的有效成分作为含量测定指标，采用高效液相色谱法进行检测，准确度高，专属性强，重现性好，能有效控制制剂质量。Objective To measure the content of Emodin and Chrysophanold in Xianghuangtongbian Capsule by using highly-effective liquid chromatography. Methods ①HPLC： The contents of Emodin and Chrysophanold were detected separately. Proper stationary phase was chosen, the makeup, matching, flow rate and column temperature of mobile phase were adjusted, in the condition of max wavelength （nm）, the absorption peaks were separated completely, the the- oretical plate number met the standard. ②Linearity range investigation： confecting reference substance solution of dif- ferent concentration, performing linear regression with chromatographic peak area as y-axis and sampling concentration as x-axis to get curvilinear regression and investigating linearity range. ③Methodological investigation： the repeatabili- ty, intermediate precision, reproducibility, durability, stability and sample recovery rate of the method were investigat- ed. ④Sample content determination： determining the content of index components in three groups of samples according to the methods mentioned above. Results The concentration of Emodin and Chrysophanold in Xianghuangtongbian Capsule was determined using a HPLC system at the wavelength of 254 nm. The separation was achieved by using a Welch Ultimate XB-C 18, at a rate of 1 mL/min. The temperature of column was 25℃. The mobile phase consisted of methyl alcohol and 0.1% Phosphoric acid at a ratio of 80：20 （V/V）, Emodin and Chrysophanold had a good linear rela- tionship among 1.4 -70, 19.8-990 μg/mL, r was all 0.9999. RSD （%） of precision, precision in middle, repeatability, durable property, the stability within 12 hours and analytical recovery for Emodin and Chrysophanold were 0.58%, 0.15%; 1.25%, 0.32%; 1.48%, 0.49%; 1.35%, 0.43%; 1.25%, 0.13%; 0.62%, 0.46%. The analytical recovery was 99.6%, 99.7%. It was no less than 3.3 nag in per granule of the total content of Emodin and Chrysophanold. Conclu-sion Regard the accepted active ingredients as a target of determining the co

关 键 词：香黄通便胶囊 含量测定 高效液相色谱法 大黄素 大黄酚 

分 类 号：R286.0[医药卫生—中药学]