摘要
目的对连钱草进行薄层鉴别和含量测定研究,提高其质量控制方法和标准。方法薄层色谱法(TLC),以熊果酸为对照品,连钱草为对照药材,以环己烷-乙酸乙酯-甲酸(3∶1∶0.1)为展开剂,以10%硫酸乙醇为显色剂;建立高效液相色谱法(HPLC)测定迷迭香酸的含量,色谱柱为waters SunFire C18(250 mm×4.6 mm,5μm),流动相为乙腈-0.1%磷酸溶液(21∶79),检测波长为330 nm,柱温为30℃,流速为1.0 mL/min。结果建立的TLC鉴别方法,斑点清晰,分离效果较好;HPLC法测定迷迭香酸在4.62~231.03μg/mL范围内线性关系良好(r=0.9999),精密度、稳定性、重复性RSD均小于1.0%;平均加样回收率为99.6%,RSD=1.16%。26批样品中迷迭香酸的含量在0.827~12.484 mg/g。结论建立的方法简便、易操作,结果准确,能有效控制连钱草的药材质量。
Objective To improve the quality standards for glechomae herba by TLC and quantitate determine.Methods Thin layer chromatography(TLC)was performed with ursolic acid as reference substances,glechomae herba as the control herb,cyclohexane-ethyl acetate-formic acid(3∶1∶0.1)as the developing solvent,and 10%ethanol sulfate as the colorimetric agent.The contents of rosmarinic acid determined by HPLC.The waters SunFire C18(250 mm×4.6 mm,5μm)was used with the mobile phase of acetonitrile-phosphoric acid solution(21∶79),at the detection wavelength was 330 nm,and the column temperature was at 30℃,the flow rate of 1.0 mL/min.Results The spots in the TLC were clear and well-separated;the linear ranges of rosmarinic acidwas 4.62-231.03μg/mL(r=0.9999),respectively.RSDs of precision,stability and repeatability tests were less than 1.0%;the average recoveries was 99.6%(RSD=1.16%).The contents of rosmarinic acidwas in 26 batches of samples were 0.827-12.484 mg/g.Conclusion The established method is simple,easy to operate with accurate results,whereby it can effectively control the quality of glechomae herba.
作者
周雷罡
马银松
喻何云
袁铭铭
吴西
ZHOU Leigang;MA Yinsong;YU Heyun;YUAN Mingming;WU Xi(Jiangxi Institute for Drug Control,NMPA Key Laboratory of Quality Evaluation of Traditional Chinese Patent Medicine,Jiangxi Province Engineering Research Center of Drug and Medical Device Quality,Nanchang Jiangxi 330029,China)
出处
《药品评价》
CAS
2023年第6期672-675,共4页
Drug Evaluation
基金
江西省药品监督管理局科研项目(2021KY19)
江西省重点研发计划项目(2017BBG70104)
2022年度国家药品标准制修订研究课题(2022Z03)。