摘要
目的建立同时测定大黄药材中的芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的方法。方法采用反相高效液相色谱(RP-HPLC)法对大黄药材中5种蒽醌及其苷的含量进行测定。色谱条件如下,色谱柱:E Merek Li Chrospher 100RP-18(4.6mm×250mm,5μm),流动相为甲醇-0.5%高氯酸(85:15),流速0.8ml/min,柱温40℃,检测波长为254nm。结果在此色谱条件下,各蒽醌成分达到基线分离,且峰形良好。芦荟大黄索线性回归方程为:Y=-2410+5374661X,r=0.9994,在0.016~0.160μg范围内呈良好线性关系,其平均回收率为104.8%,RSD=1.65%;大黄酸线性回归方程为Y=2148+5440831x,r=0.9997,在0.012—0.120μg范围内呈良好线性关系,其平均回收率为104.0%,RSD=2.71%;大黄素线性回归方程为Y=1653+4923143X,r=0.9998,在0.017—0.166lag范围内呈良好线性关系,其平均回收率为101.4%,RSD=1.86%;大黄酚线性回归方程为Y=5823+6496978X,r=0.9998.在0.029—0.286lag范围内呈良好线性关系.其平均回收率为103.2%,RSD=1.93%;大黄素甲醚线性回归方程为Y=3827+3385073X.r=0.9996,在0.008—0.079Ixg范围内呈良好线性关系,其平均回收率为102.0%,RSD=1.85%。结论分析方法快速、灵敏、准确,所有待测组分峰分离度良好,达到定量检测的要求。
Objective To develop an HPLC method for determination of the Rhubarb anthraquinones ( Aloe - emodin, Rhein, Emodin, Chrysophanol, Physcion and their conjunctive compounds) in Radix et Rh/zoma Rhei. Methods Rhubarb anthraquinones were simultaneously separated and determined on a Merck Chrospher 100RP-18 column (250 mm× 4.6 mm, 5μm) . The detective wavelength was 254 nm. The mobile phase consisted of methanol-0. 5% HC104 (85: 15) and the flow rate was 0. 8 ml · min^-1. Results Under the chromatographic condition, the five compounds were completely separated and other components had no effect on their determination. Every Rhubarb anthraquinoneg calibration curve, correlation coefficient, linearity range and average recoveries showed respectively as followed:①Aloe - emodin berberine : Y = - 2 410 + 5 374 661X, r = 0. 999 4, linearity range 0.016 - 0. 160 0,g, the average recovery 104.8% ,RSD = 1.65 %.②Rhein berberine: Y = 2 148 + 5 440 831 X, r = 0. 999 7, lineari ty range 0.012 - 0.120 μg, the average recovery 1 04.0%, RSD = 2.71%. ③Etnodin berberine: Y = 1 653 + 4 923 143X, r = 0. 999 8, linearity range 0. 017 -0. 166μg, the average recovery 101.4% ,RSD = 1.86%. ④ Chrysophanol berberine: Y=5 823 + 6 496 978X, r = 0. 999 8,1inearity range 0. 029 - 0. 286 μg, the average recovery 103.2%, RSD = 1.93%. ⑤Physcion berberine: Y=3 827 +3 385 073X,r =0.999 6,1inearity range 0.008 -0.079 μg, the average recovery 102.0% ,RSD = 1.85%. Conclusion The method is simple, accurate, rapid and sensitive. Key words:Radix et Rhizoma Rhei; Content determination; HPLC
出处
《时珍国医国药》
CAS
CSCD
北大核心
2006年第7期1201-1202,共2页
Lishizhen Medicine and Materia Medica Research
关键词
大黄
含量测定
高效液相色谱
Radix et Rhizoma Rhei
Content determination
HPLC