HPLC法同时测定中药五灵脂中3种成分的含量

目的建立同时测定五灵脂中原儿茶酸、穗花杉双黄酮和扁柏双黄酮含量的方法,为五灵脂的质量控制和开发利用提供依据。方法采用HPLC法,色谱柱:Diamonsil ODS C18柱(250 mm×4.6 mm,5μm),流动相:乙腈(A)-体积分数为0.5%的冰醋酸溶液(B),梯度洗脱程序:0~15 min:85%~65%(B)、15~35 min:65%~40%(B)、35~40 min:40%~25%(B)、40~60 min:25%~10%(B)、60~65 min:10%~0%(B),流速:0.8 mL.min-1,检测波长:265 nm,柱温:室温。结果原儿茶酸、穗花杉双黄酮和扁柏双黄酮其质量分别在0.0496~0.4960(r=0.9998)、0.1260~1.2600(r=0.9999)和0.0985~0.9850μg(r=0.9996)内与其峰面积呈良好线性关系,平均回收率分别为100.4%、99.7%和101.2%,RSD分别为2.3%、2.1%和2.0%。结论所建立的方法可用于五灵脂的质量控制。

Determination of protocatechuic acid, amentoflavone and hinokiflavone in faeces trogopterori by HPLC

Objective To provide basis for the quality control and exploitation of Faeces Trogopterori (FT), and establish an HPLC method for simultaneous determination of protocatechuic acid, amentoflavone and hinokiflavone in this drug. Methods The separation and quantification of three constituents above were performed on a Diamonsil ODS C₁₈ (250 mm×4.6 mm, 5 μm) ; the mobile phase consisted of acetonitrile(A) ~ 0.5% aqueous acetic acid(B) with an optimized gradient program of 0-15 min: 85%-65% (B), 15-35 min: 65%-40% (B), 35-40 min: 40%-25% (B), 40-60 min: 25%-10% ( B), 60-65 min: 10%-0 (B), with a flow rate of 0.8 mL·min^-1 ; the wavelength was set at 265 nm. The experiment was performed under room temperature. Results Protocatechuic acid, amentoflavone and hinokiflavone showed good separation with method above. The linear ranges was 0.049 6-0.496 0 μg (r = 0.999 8) for protocatechuic acid, 0.126 0-1.260 0 μg (r = 0.999 9) for amentoflavone and 0.098 5-0.985 0 μg (r = 0.999 6) for hinokiflavone. The mean recoveries for these three standard substances were 100.4 %, 99.7 % and 101.2 % with RSD of 2.3 %, 2.1 % and 2.0 %, respectively. Conclusions The established method is accurate and simple which could be used for the quality control of FT.