目的 建立HPLC-DAD法同时测定精制冠心片中丹参酮II_A、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,Zorbax Eclipse XDB-C₁₈色谱柱(250 mm×4.6 mm,5.0 μm),甲醇-乙腈(25:75,A)-0.1%甲酸水溶液(B)为流动相,体积流量1.0 mL/min,梯度洗脱: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;分段变波长测定:0～19.0 min为270 nm,19.0～22.0 min为230 nm,22.0～27.0 min为320 nm,27.0～40.0 min为402 nm;柱温30 ℃;进样量10 μL。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II_A在0.4～8.0 mg/L(r=0.999 5)、芍药苷在1.2～24.0 mg/L(r=0.999 1)、丹酚酸B在3.2～64.0 mg/L(r=0.999 3)、阿魏酸在0.08～1.60 mg/L(r=0.999 5)、红花黄色素A在1.2～24.0 mg/L(r=0.999 3)、藁本内酯在0.24～4.80 mg/L(r=0.999 7)、丹参素在0.32～6.40 mg/L(r=0.999 7)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12 h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II_A在0.704～0.797 mg/g,芍药苷在3.124～3.411 mg/g,丹酚酸B在7.129～7.611 mg/g,阿魏酸在0.180～0.198 mg/g,红花黄色素A在2.718～2.966 mg/g,藁本内酯在0.590～0.683 mg/g,丹参素在0.811～0.899 mg/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 II_A, paeoniflorin, salvianolic acid B, ferulic acid, safflor 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 μm) 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 min was 320 nm, 27.0—40.0 min 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 II_A 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), safflor 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, safflor 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.