百合知母汤有效部位质量控制方法研究

Quality Control of Effective Fraction in Baihe Zhimu Decoction

目的:建立百合知母汤中知母黄酮类成分芒果苷、皂苷类成分知母皂苷A3,百合酚类成分咖啡酰基甘油酯、皂苷类成分麦冬皂苷D’质量控制方法。方法:采用HPLC-DAD分析方法,依利特Hypersil ODS色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.1%磷酸水溶液为流动相梯度洗脱,流速1 mL.min-1,检测波长芒果苷为258 nm,知母皂苷A3为191 nm,咖啡酰基甘油酯为310 nm,麦冬皂苷D’为200 nm,柱温25℃。结果:芒果苷,咖啡酰基甘油酯,知母皂苷A3,麦冬皂苷D’分别在0.228～1.14,0.072～0.576,0.069 25～0.554,0.101～0.505 g.L-1线性关系良好;平均回收率分别为98.97%,99.32%,97.65%,96.67%。芒果苷的定量限为0.912 mg.L-1,检测限为0.456 mg.L-1;咖啡酰基甘油酯的定量限为1.44 mg.L-1,检测限为0.36 mg.L-1;知母皂苷A3的定量限为5.54 mg.L-1,检测限为1.85 mg.L-1;麦冬皂苷D’定量限为3.16 mg.L-1,检测限为1.06 mg.L-1。结论:3批样品含量测定结果表明,该方法简便、准确,可用于百合知母汤中芒果苷、咖啡酰基甘油酯、知母皂苷A3和麦冬皂苷D’的含量测定,亦可作为百合知母汤质量控制方法之一。

Objective： To find a quality control method of mangiferin, anemarrhena saponin A3, caffeoyl glyceride and ophiopogonin D, which are flavones effective fraction, steroidal saponins effective fraction from Zhimu （Anemarrhenae Rhizoma） , the total phenylic effective fraction and steroidal saponins effective fraction from Baihe （Lilium lancifolium ） in Baihe Zhimu decoction respectively. Method： The procedure of HPLC-DAD was performed on the chromatographic column of Yi li-te Hypersil ODS （4.6 mm x 250 ram, 5 p,m） at 25 ~C. The mobile phase was acetonitrile-0. 1% phosphoric acid solution in gradient elution. The flow velocity was 1.0 mL ~ min i and the detection wavelength was set at 258 nm for mangiferin, 191 nm for anemarrhena saponin A3, 310 nm for caffeoyl glyceride and 200 nm for ophiopogonin D＇. Result： Mangiferin showed a good linear relationship in a range from 0. 228-1.14 g L-1 ; caffeoyl glyceride from 0. 072-0. 576 g L- 1, anemarrhena saponin A3 from 0. 069 25-0. 554 g L-l , ophiopogonin D＇ from 0. 101-0. 505 g L-1. The average recovery was 98.97% , 99.32% , 97.65% and 96.67% respectively. The limit of quantitation and detection about mangiferin was 0. 912 mg L-1 and 0. 456 mg L-1. The LOQ and LOD about caffeoyl glyceride was 1.44, 0.36 mg L 1 The LOQ and LOD about anemarrhena saponin A3 was 5.54, 1.85 mg L-1. The LOQ and LOD about ophiopogonin D＇ was 3.16, 1.06 mg determination of control of Baihe L - 1. Conclusion ： mangiferin, caffeoyl Zhimu decoction. The method was simple glyceride ; anemarrhena and reliable, which can be used sapon!n A3 and ophiopogonin for the quantitative as well as quantity