肋柱花的定性定量分析  

Qualitative and quantitative analysis for Lomatogonium rotatum

作　　者：包文林 张朝鲁孟 王美丽[1] 辛颖[1] 王青虎[1] BAO Wenlin;ZHANG Chaolumeng;WANG Meili;XIN Ying;WANG Qinghu(College of Traditional Mongolian Medicine,Inner Mongolia University for Nationalities,Tongliao 028000,China)

机构地区：[1]内蒙古民族大学蒙医药学院,内蒙古通辽028000

出　　处：《中国药品标准》2023年第5期481-487,共7页Drug Standards of China

基　　金：国家重点研发计划资助(2019YFC1712303);内蒙古自然科学基金项目(2021MS08070);内蒙古自治区卫生健康委医疗卫生科技计划项目(2021MS08070)。

摘　　要：目的:研究肋柱花TLC鉴别及多成分同时测定的方法。方法:利用TLC法对肋柱花中1,8-二羟基-4,6-二甲氧基双苯吡酮、1,3,5,8-四羟基-5,6,7,8-四氢双苯吡酮、乌苏酸和獐牙菜苦苷进行色谱鉴别。采用HPLC法对不同批次肋柱花进行含量测定,色谱柱为Topsil C_(18)柱(4.6 mm×250 mm,5μm);以乙腈(A)-水(B)为流动相,梯度洗脱(B;0~15 min,85%→75%;15~30 min,75%→55%)。流速为1.0 mL·min^(-1),柱温40℃,进样量10μL。獐牙菜苦苷为237 nm,而异牡荆苷、当药黄素和当药醇苷为275 nm。结果:1,8-二羟基-4,6-二甲氧基双苯吡酮和1,3,5,8-四羟基-5,6,7,8-四氢双苯吡酮以石油醚-丙酮-甲酸(5∶1∶0.2)为展开剂,而乌苏酸和獐牙菜苦苷分别以环己烷-乙酸乙酯-冰醋酸(10∶2∶0.3)和二氯甲烷-甲醇-甲酸(5∶1∶0.1)为展开剂时,斑点清晰,Rf值符合要求。在选用色谱条件下,被检测成分在较宽浓度范围内呈良好的线性关系(r>0.9994)。其平均回收率分别为98.47%、96.44%、97.80%和96.52%,RSD分别为0.49%、1.6%、1.4%和1.5%。结论:创建了肋柱花的定性定量分析方法,为综合评价该药材质量提供依据。Objective:To investigate on the TLC identification and multi-component simultaneous determination method for Lomatogonium rotatum.Methods:The 1,8-dihydroxy-4,6-dimethoxyxanthone,1,3,5,8-tetrahydroxy-5,6,7,8-tetrahydroxanthone,ursolic acid and swertiamarin were identified by TLC.HPLC was adopted to determine the content of different batches of Lomatogonium rotatum.Topsil C_(18) column(4.6 mm×250 mm,5μm)was used with acetonitrile(A)-water(B)as mobile phase on gradient elution(B;0-15 min,85%→75%;15-30 min,75%→55%)at the flow rate of 1.0 mL·min^(-1).The column temperature was 40℃and the injection volume was 10μL.Detection wavelength was set at 237 nm for swertiamarin and at 275 nm for isovitexin,swertisin and swertianolin.Results:When 1,8-dihydroxy-4,6-dimethoxyxanthone and 1,3,5,8-tetrahydroxy-5,6,7,8-tetrahydroxanthone were developed with petroleum ether-acetone-formic acid(5∶1∶0.2),and ursolic acid and swertiamarin were developed with cyclohexane-ethyl acetate-glacial acetic acid(10∶2∶0.3)and dichloromethane-methanol-formic acid(5∶1∶0.1),respectively,the spots of detected components were clear and their Rf values met the requirements.Under the selected chromatographic conditions,the detected components showed good linearity(r>0.9994)in a wide concentration range.Their average recoveries were 98.47%,96.44%,97.80%and 96.52%,respectively,and the RSDs were 0.49%,1.6%,1.4%and 1.5%,respectively.Conclusion:The qualitative and quantitative analysis method for Lomatogonium rotatum provides a basis for the comprehensive evaluation of the quality of the medicinal material.

关 键 词：肋柱花 高效液相色谱法 薄层色谱法 双苯吡酮 獐牙菜苦苷 同时测定 

分 类 号：R921.2[医药卫生—药学]