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目的:建立同时测定精制冠心颗粒中丹参素、丹酚酸B、原儿茶醛、芍药苷和阿魏酸含量的方法。方法:采用高效液相色谱法。色谱柱为 Zorbax Eclipse XDB-C18,流动相为乙腈-甲醇-0.5%磷酸(梯度洗脱),流速为1.0 ml/min,检测波长为280 nm(丹参素、原儿茶醛、丹酚酸B)、230 nm(芍药苷)、320 nm(阿魏酸),柱温为30 ℃,进样量为1.0 μl。结果:丹参素、原儿茶醛、丹酚酸B、芍药苷和阿魏酸检测质量浓度线性范围分别为1.19~478.34 μg/ml(r=0.999 9)、0.11~44.93 μg/ml(r=0.999 9)、7.49~995.20 μg/ml(r=0.999 7)、0.95~379.39 μg/ml(r=0.999 9)、0.01~3.12 μg/ml(r=0.999 5);定量限分别为1.91、0.36、150.00、2.74、0.10 ng,检测限分别为0.96、0.10、45.00、1.52、0.03 ng;精密度、稳定性、重复性试验的RSD<2%;加样回收率分别为98.06%~99.47%(RSD=0.52%,n=6)、98.01%~99.49%(RSD=0.70%,n=6)、98.44%~99.45%(RSD=0.37%,n=6)、96.94%~100.71%(RSD=1.27%,n=6)、95.44%~100.44%(RSD=1.90%,n=6)。结论:该方法操作简单、结果准确,适用于同时测定精制冠心颗粒中丹参素、原儿茶醛、丹酚酸B、芍药苷和阿魏酸的含量。
OBJECTIVE: To establish a method for simultaneous determination of danshensu, salvianolic acid B, protocatechuic aldehyde, paeoniflorin and ferulic acid in Jingzhi guanxin granule. METHODS: HPLC was performed on the column of Zorbax Eclipse XDB-C18 with mobile phase of acetonitrile-methanol -0.5% H3PO4(gradient elution) at a flow rate of 1.0 ml/min, the detection wavelength was 280 nm (for danshensu, protocatechuic aldehyde, salvianolic acid B),230 nm (for ferulic acid) and 320 nm (for paeoniflorin), column temperature was 30 ℃,injection volume was 10 μl. RESULTS: The linear range was 1.19-478.34 μg/ml for danshensu(r=0.999 9), 0.11-44.93 μg/ml for protocatechuic aldehyde(r=0.999 9),7.49-995.20 μg/ml for salvianolic acid B(r=0.999 7), 0.95-379.39 μg/ml for paeoniflorin (r=0.999 9) and 0.01-3.12 μg/ml for ferulic acid (r=0.999 5); the limits of quantitation were 1.91 ng, 0.36 ng, 150.00 ng, 2.74 ng and 0.10 ng, limit of detection were 0.96 ng, 0.10 ng,45.00 ng,1.52 ng and 0.03 ng; RSDs of precision, stability and reproducibility tests were lower than 2%; recoveries were 98.06%-99.47% (RSD=0.52%,n=6), 98.01%-99.49% (RSD=0.70%,n=6), 98.44%-99.45% (RSD=0.37%,n=6), 96.94%-100.71% (RSD=1.27%,n=6) and 95.44%-100.44% (RSD=1.90%,n=6). CONCLUSIONS: The method is simple and accurate, and suitable for the simultaneous determination of danshensu, salvianolic acid B, protocatechuic aldehyde, paeoniflorin and ferulic acid in Jingzhi guanxin granule.
含量测定高效液相色谱法丹参素原儿茶醛丹酚酸B芍药苷阿魏酸
Content determinationHPLCDanshensuProtocatechuic aldehydeSalvianolic acid BPaeoniflorinFerulic acid
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