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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,Zorbax Eclipse XDB-C18色谱柱(250 mm×4.6 mm,5.0μm),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 m L/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10μL。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0.4~8.0 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IIA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 establish a HPLC-DAD method for the simultaneous determination of seven components of tanshinone IIA, paeoniflorin, salvianolic acid B, ferulic acid, safflower yellow pigment A, ligustilide, and danshensu in refined Guanxin Pian. Methods HPLC was performed on a Zorbax Eclipse XDB-C18 column (250 mm × 4.6 mm, 5.0 μm) with a mobile phase of methanol-acetonitrile (25:75, A) -0.1% formic acid in water / min, gradient elution: 0 to 10.0 min, 95% B; 10.0 to 16.0 min, 95% to 85% B; 16.0 to 18.0 min, 85% B; 18.0 to 22.0 min, 85% to 75% B; ~ 26.0 min, 75% ~ 65% B, 26.0 ~ 40.0 min and 65% ~ 15% B, respectively. 320 nm, 27.0 ~ 40.0 min to 402 nm; column temperature 30 ℃; injection volume 10μL. The linear relationship, precision, repeatability, stability and sample recovery were investigated. Results The results showed that tanshinone IIA of 7 kinds of index components were 0.4 ~ 8.0 mg / L (r = 0.999 5), paeoniflorin was 1.2 ~ 24.0 mg / L (r = 0.999 1) = 0.999 3), ferulic acid was in the range of 0.08-1.60 mg / L (r = 0.999 5), safflower A was 1.2-24.0 mg / L (r = 0.999 3), ligustilide was in the range of 0.24-4.88 mg /L(r=0.9997). The linearity of Danshensu was good at 0.32-6.40 mg / L (r = 0.999 7). The precision was good with RSD less than 2.0%. The reproducibility was good with RSD less than 2.0% Under 12 h, the average recovery was 98.05% ~ 101.27%, RSD was less than 2.0%. The content of tanshinone IIA in 6 batches of samples 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, Pigment A was 2.718 ~ 2.966 mg / g, ligustilide was 0.590 ~ 0.683 mg / g, Danshensu was 0.811 ~ 0.899 mg / g. Conclusion The method is simple, accurate and reproducible. It provides experimental evidence for the quality control of refined capitatum tablets.