摘要
目的建立HPLC—DAD法同时测定精制冠心片中丹参酮IIA、芍药苷、丹酚酸B、阿魏酸、红花黄色素A、藁本内酯、丹参素7种指标成分的量。方法采用HPLC法，ZorbaxEclipseXDB—C18色谱柱（250mm×4．6mm，5．0gm），甲醇．乙腈（25：75，A）．0．1％甲酸水溶液（B）为流动相，体积流量1．0mL／min，梯度洗脱：0～10．0min，95％B；10．0～16．0min，95％～85％B；16．0～18．0min，85％B；18．O～22．0min，85％～75％B；22．0～26．0min，75％～65％B，26．0～40．0min，65％～15％B；分段变波长测定：0～19．0min为270mm，19．0～22．0min为230nm，22．O～27．0min为320nm，27．0～40．0min为402nm；柱温30℃；进样量10此。分别对线性关系、精密度、重复性、稳定性及加样回收率进行考察。结果7种指标成分丹参酮IIA在0．4～8．0mg／L（r=0．9995）、芍药苷在1．2～24．0mg／L（r=0．9991）、丹酚酸B在3．2～64．0mg／L（r=0．9993）、阿魏酸在O．08～1．60mg／L（r=0．9995）、红花黄色素A在1.2～24．0mg／L（r=0．9993）、藁本内酯在0．24～4．80mg／L（r=0．9997）、丹参素在0．32～6．40mg/L（r=0．9997）线性关系良好；精密度良好，RSD均小于2．0％；重复性良好，RSD均小于2．0％；在室温条件下12h内稳定；平均加样回收率在98．05％～101．27％，RSD均小于2．0％。6批样品中丹参酮IIA在0．704～0．797mg／g，芍药苷在3．124～3．411mg／g，丹酚酸B在7．129～7．611mg／g，阿魏酸在0．180～0．198mg／g，红花黄色素A在2．718～2．966mg／g，藁本内酯在0．590～0．683mg／g，丹参素在0．811～0．899mg／g。结论该方法简便、准确，重复性好，为精制冠心片的质量控制提供实验依据。
Objective To develop an HPLC method for the simultaneous determination of tanshinone IIA, paeoniflorin, salvianolic acid B, ferulic acid, saffior yellow A, ligustilide, and danshensu in Refined Coronary Tablets. Methods The chromatographic separation was achieved on a Zorbax Eclipse XDB-C18 column （250 mm × 4.6 mm, 5.0 mm） with methanol-acetonitrile （25 ： 75, A）-0.1% formic acid （B） as mobile phases at the flow rate of 1.0 mL/min for gradient elution： 0-10.0 min, 95% B; 10.0-16.0 min, 95%-85% B; 16.0-18.0 min, 85% B; 18.0-22.0 min, 85%-75% B; 22.0-26.0 min, 75%-65% B; 26.0-40.0 min, 65%-15% B; Detection with variable wavelength： 0-19.0 min was 270 nm, 19.0-22.0 min was 230 nm, 22.0-27.0 rain was 320 nm, 27.0- 40.0 rain was 402 nm, and the column temperature was 30 ℃. Its linear relationship, precision, repeatability, stability, and recoveries were investigated. Results The results showed that the seven active components were well separated and showed good linearity,tanshinone IIA 0.4-8.0 mg/L （r = 0.999 5）, paeoniflorin 1.2-24.0 mg/L （r = 0.999 1）, salvianolic acid B 3.2-64.0 mg/L （r = 0.999 3）, ferulic acid 0.08-1.60 mg/L （r = 0.999 5）, saffior yellow A 1.2-24.0 mg/L （r = 0.999 3）, ligustilide 0.24-4.80 mg/L （r = 0.999 7）, and danshensu 0.32-6.40 mg/L （r = 0.999 7）. The precision was good, and RSD was less than 2.0%. The repeatability was good, and RSD was less than 2.0%. The stability was good in 12 h. The average recoveries were between 98.05%-101.27%, and RSD was less than 2.0%. The contents of target components in Refined Coronary Tablets, tanshinone was 0.704-0.797 mg/g, paeoniflorin was 3.124-3.411 mg/g, salvianolic acid B was 7.129-7.611 mg/g, ferulic acid was 0.180-0.198 mg/g, saffior yellow A was 2.718- 2.966 mg/g, ligustilide was 0.590-0.683 mg/g, and danshensu was 0.811-0.899 mg/g. Conclusion The method is accurate, sensitive, credible, and repeatable. It can be applied to the quality control of Refined Coronary Tablets.
出处
《中草药》
CAS
CSCD
北大核心
2015年第14期2092-2095,共4页
Chinese Traditional and Herbal Drugs
