石斛甲醇提取物HPLC-MS分析及4种多酚测定

目的 采用HPLC-MS法分析石斛甲醇提取物及测定丁香酸、氧化白藜芦醇、芦丁和柚皮素的含有量.方法 石斛甲醇溶液的分析采用SinoChrome ODS-AP色谱柱(4.6 mm×250 mm,5μm);流动相甲醇-0.2%醋酸水,梯度洗脱;体积流量0.5 mL/min;柱温25℃;检测波长334 nm.电喷雾离子源(ESI),负离子模式下采集数据.结果 丁香酸、氧化白藜芦醇、芦丁、柚皮素分别在0.27~8.54 μg/mL(r=0.9995)、1.25~40.03 μg/mL(r=0.9993)、1.25 ~ 40.00 μg/mL(r=0.999 3)、2.70~ 86.70 μg/mL(r=0.999 6)范围内线性关系良好,平均加样回收率分别为100.63%(RSD=1.35%)、99.72%(RSD=1.63%)、100.04% (RSD=1.12%)、99.95%(RSD=2.16%).不同样品中多酚含有量存在一定差异,其中霍山石斛含有量最高.结论 该方法准确、简便、重复性好,可用于石斛药材的质量控制.

Analysis of methanol extract from Dendrobii Caulis by HPLC MS and determi nation of four polyphenols

AIM To analyze the methanol extract from Dendrobii Caulis by HPLC MS and to determine the contents of syringic acid,oxidized resveratrol,rutin and naringenin.METHODS The analysis of methanol extract of Dendrobii Caulis was performed on a 25℃thermostatic SinoChrome ODS AP column(4.6 mm×250 mm,5μm),with the mobile phase comprising of methanol 0.2%acetic acid flowing at 0.5 mL/min in a gradient elution manner,and the detection wavelength was set at 334 nm.The data were collected in negative ion mode using electron spray with ESI source.RESULTS The syringic acid,oxidized resveratrol,rutin and naringenin showed good linear relationships within the ranges of 0.27 8.54μg/mL(r=0.9995),1.25 40.03μg/mL(r=0.9993),1.25 40.00μg/mL(r=0.9993),2.70 86.70μg/mL(r=0.9996),whose average recoveries were 100.63%(RSD=1.35%),99.72%(RSD=1.63%),100.04%(RSD=1.12%),99.95%(RSD=2.16%),respectively.The content of polyphenols in different samples were significantly different,with the highest content polyphenols in Dendrobium huoshanense C.Z.Tang et S.J.Cheng.CONCLUSION This accurate,stable and reproducible method can be used for the quality control of Dendrobii Caulis.