摘要
建立医院制剂薏仁祛湿合剂的质量标准与提取工艺研究方法。采用薄层色谱法(TLC)做定性鉴别,分别鉴定薏仁祛湿合剂中含有的石菖蒲和石斛2味药材;采用正交设计法以加水倍量、煎煮时间、提取次数为因素,以薏仁祛湿合剂提取液中石斛酚的含量为指标,优选最佳的水提工艺。色谱条件:色谱柱为Gemini®-C_(18)110Å(5µm,4.6 mm×250 mm),流动相为甲醇(A)-0.1%磷酸水溶液(B),梯度洗脱;流速:1.0 mL/min;柱温:30℃;检测波长:230 nm;进样量:10µL。TLC鉴别出薏仁祛湿合剂中石菖蒲和石斛2味药材,且特征斑点稳定性良好、清晰。最佳水提工艺为:加8倍量水煎煮1 h,提取2次。石斛酚浓度在0.021 31~0.127 86 mg/mL范围之内呈良好的线性关系,平均加样回收率为98.54%的,RSD值2.46%,精密度高,稳定性及重复性的RSD<3%,说明试验方法可靠。TLC和HPLC作为薏仁祛湿合剂的质量控制方法,准确度高、重复性好,为薏仁祛湿合剂的质量控制奠定了基础。
The quality standard and extraction process of hospital preparation Yiren Qushi Mixture was established.Thin layer chromatography(TLC)was used for qualitative identification to identify two medicinal materials of Acorus tatarinowii Schott and Dendrobium in Yiren Qushi Mixture.The orthogonal design method was used to optimize the water extraction process with the amount of water,decoction time and extraction times as the factors,and the content of gigantol in the extract of Yiren Qushi Mixture as the index.Chromatographic conditions were as follows:chromatographic column was Gemini®-C_(18)110Å(5μm,4.6 mm×250 mm),mobile phase was methanol(A)-0.1%phosphoric acid aqueous solution(B),with gradient elution,flow rate was 1.0 mL/min,column temperature was 30℃,detection wavelength was 230 nm,injection volume was 10μL.TLC identified two medicinal materials of Acorus tatarinowii Schott and Dendrobium in Yiren Qushi Mixture,and the characteristic spots were stable and clear.The best water extraction process was as follows:adding 8 times the amount of water decoction 1 h,extracted twice.The concentration of gigantol showed a good linear relationship in the range of 0.02131 to 0.12786 mg/mL.The average recovery rate was 98.54%,and RSD value was 2.46%.The precision was high,and RSD of stability and repeatability was less than 3%,indicating that the test method was reliable.TLC and HPLC,as the quality control methods of Yiren Qushi Mixture,had high accuracy and good repeatability,which laid a foundation for the quality control of Yiren Qushi Mixture.
作者
魏江存
杨绘霖
青冰
黄琳云
彭宪
李凤珍
钟文
WEI Jiangcun;YANG Huilin;QING Bing;HUANG Linyun;PENG Xian;LI Fengzhen;ZHONG Wen(Guangxi International Zhuang Medicine Hospital,Guangxi Nanning 530201,China)
出处
《广州化工》
2025年第24期60-63,161,共5页
GuangZhou Chemical Industry
基金
广西科技厅重点研发计划(No.桂科AB21196057)
广西壮族自治区中医药管理局自筹科研课题项目(No.GXZYA20220141、GXZYA20220142)
广西国际壮医医院“青苗工程”人才培育项目(2022001)
国家中医药管理局全国老药工传承工作室建设项目[钟文](国中医药人教函[2024] 255号)
国家中医药管理局高水平中医药重点学科建设项目-少数民族药学(壮药学)[zyyzdxk-2023165]
广西中医药多学科交叉创新团队项目(GZKJ2309)
广西中医药大学“高层次人才培育创新团队”资助项目(2022A008)。
关键词
薏仁祛湿合剂
质量分析
薄层色谱鉴别
含量测定
coix seed dampness expelling mixture
quality analysis
TLC identification
content determination
