摘要
目的:结合固相萃取法建立滋肾育胎丸中的何首乌、续断、巴戟天和白术的薄层色谱鉴别方法。方法:采用C18固相萃取法,将供试品甲醇超声提取、蒸干、复溶后上样至活化后的固相小柱中,先后用水和不同浓度甲醇洗脱,洗脱速度为1 mL·min^(-1)。收集水洗脱液,蒸干复溶作为巴戟天鉴别供试品溶液,以三氯甲烷-甲醇-水-冰醋酸(7∶3∶1∶1)为展开剂;收集60%甲醇水洗脱液,蒸干复溶作为续断鉴别供试品溶液,以正丁醇-醋酸-水(4∶1∶5)的上层溶液为展开剂;收集80%甲醇水洗脱液,蒸干复溶作为何首乌鉴别供试品溶液,以环己烷-二氯甲烷-乙酸乙酯-甲酸(10∶1∶1∶0.1)为展开剂;收集100%甲醇洗脱液,蒸干复溶作为白术鉴别供试品溶液,以正己烷-乙酸乙酯-甲酸(40∶10∶0.5)为展开剂。结果:供试品溶液在与对照药材或对照品相应的位置上,显示相同颜色的荧光斑点,阴性样品无干扰。结论:固相萃取可以有效的将滋肾育胎丸中含量低专属性成分进行富集分析,所建立的方法具有操作简单、重复性好等特点,可用作滋肾育胎丸的薄层色谱鉴别。
Objective:To establish a thinlayer chromatographic method which combine with solid-phase extraction for the identification of Polygoni Multiflori Radix,Dipsaci Radix,Morindae Officinalis Radix and Atractylodis Macrocephalae Rhizoma in Zishen Yutai pills.Methods:C_(18)solid phase extraction was used.The sample wasloaded into the activated solidphase column after ultrasonic extraction,steam drying and redissolution of methanol.It was eluted with water and methanol of different concentrations successively,and the elution rate was 1 mL·min^(-1).The water washing was collected,evaporated the filtrate to dryness and dissolved the residue in 1 mL of methanol to produce the test solution of Morindae Officinalis Radix,a mixture of chloroform,methanol,water and glacial acetic acid(7∶3∶1∶1)was used as the mobile phase;60%methanol eluent was collected,evaporated the filtrate to dryness and dissolved the residue in 1 ml of methanol to produce the test solution of Dipsaci Radix identification,a mixture of upper layer solution of n-butanol,acetic acid and water(4∶1∶5)was used as the mobile phase;80%methanol eluent was collected,evaporated the filtrate to dryness and dissolved the residue in 1 mL of methanol to produce the test solution of Polygoni Multiflori Radix,a mixture of Cyclohexane,dichloromethane,ethyl acetate,formic acid(10∶1∶1∶0.1)was used as the mobile phase;100%methanol eluent was collected,evaporated the filtrate to dryness and dissolved the residue in 1 mL of methanol to produce the test solution of Atractylodis Macrocephalae Rhizoma,n-hexane,ethyl acetate,formic acid(40∶10∶0.5)was used as the mobile phase.Results:The fluorescent spots in the chromatogram obtained with the test solution correspond in position and colour to the spots in the chromatogram obtained with the reference drug solution and reference solution,negative samples without interference.Conclusion:Solid phase extraction can effectively enrich and analyze the low-specific components in Zishen Yutai pills.The established method has the characteristics of simple operation and good repeatability,and can be used as thin layer chromatography identification of ZishenYutai pills.
作者
唐哲
戴胜云
王蔚
宁娜
雷婷
何子昕
乔菲
郑健
马双成
TANG Zhe;DAI Sheng-yun;WANG Wei;NING Na;LEI Ting;HE Zi-xin;QIAO Fei;ZHENG Jian;MA Shuang-cheng(National Institutes for Food and Drug Control,Bejing 102629,China;China Pharmaceutical University,Nanjing 211198,China;Guangzhou Baiyunshan Zhongyi Pharmaceutical Co.,Ltd.,Guangzhou 510530,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2022年第8期1306-1311,共6页
Chinese Journal of Pharmaceutical Analysis
关键词
滋肾育胎丸
质量标准
固相萃取
薄层色谱法
何首乌
续断
巴戟天
白术
Zishen Yutai pills
quality standard
solid phase extraction
TLC
Polygoni Multiflori Radix
Dipsaci Radix
Morindae Officinalis Radix
Atractylodis Macrocephalae Rhizoma
作者简介
通信作者:马双成,Tel:(010)53852076,E-mail:mashuangcheng@nifdc.org.cn;通信作者:郑健,Tel:(010)53852080,E-mail:zhengjian@nifdc.org.cn;第一作者:唐哲,Tel:(010)53852080,E-mail:1521835783@qq.com;第一作者:戴胜云,Tel:(010)53852078,E-mail:daisy@nifdc.org.cn。
