摘要
目的提升益气健脾口服液的质量标准。方法采用薄层色谱法对制剂中的鸡内金、莲子进行定性鉴别;采用固相萃取-高效液相色谱法测定制剂中枸橼酸的含量,色谱柱为GL Sciences InerSustain AQ-C_(18)柱(250 mm×4.6 mm,5μm),流动相为0.04%庚烷磺酸钠溶液(用磷酸调pH至2.3)-乙腈(99∶1,V/V),流速为0.5 mL/min,检测波长为210 nm,柱温为35℃,进样量为10μL。结果鸡内金、莲子药材的薄层色谱斑点清晰,分离度好,且阴性对照无干扰。枸橼酸的质量浓度在0.1026~5.1306 mg/mL范围内与峰面积线性关系良好(r=1.0000,n=6);精密度、稳定性、重复性试验结果的RSD均小于1.5%;平均回收率为97.71%,RSD为0.86%(n=9)。15批样品的枸橼酸含量为5.82~10.90 mg/mL。结论该方法操作简便、专属性强、重复性好、结果准确,可用于益气健脾口服液的质量控制。拟定限度为每1 mL制剂中含有机酸以枸橼酸(C_(6)H_(8)O_(7))计应不得少于4.0 mg。
Objective To improve the quality standard of Yiqi Jianpi Oral Liquid.Methods Thin-layer chromatography(TLC)method was used to qualitatively identify Galli Gigerii Endothelium Corneum and Nelumbinis Semen in the preparation.High-performance liquid chromatography(HPLC)method was used to determine the content of citric acid in the preparation by solid-phase extraction.The chromatographic column was GL Sciences InerSustain AQ-C_(18) column(250 mm×4.6 mm,5μm),and the mobile phase was 0.04%sodium heptanesulfonate solution(adjusted to pH 2.3 with phosphoric acid)-acetonitrile(99∶1,V/V),the flow rate was 0.5 mL/min,the detection wavelength was 210 nm,the column temperature was 35℃,and the injection volume was 10μL.Results The TLC spots of Galli Gigerii Endothelium Corneum and Nelumbinis Semen were clear,with good separation and no interference from the negative control.The linear range of citric acid was 0.1026-5.1306 mg/mL(r=1.0000,n=6).The RSDs of precision,stability,and repeatability test results were all lower than 1.5%.The average recovery of citric acid was 97.71%,with an RSD of 0.86%(n=9).The content of citric acid in 15 batches of samples was in the range of 5.82-10.90 mg/mL.Conclusion The method is simple,highly specific,with good reproducibility,and accurate results,which can be used for quality control of Yiqi Jianpi Oral Liquid.The proposed limit is that the content of citric acid(C_(6)H_(8)O_(7))in 1 mL preparation should not be lower than 4.0 mg.
作者
郑文燕
连晓吟
陈佩文
刘珍
刘潇潇
ZHENG Wenyan;LIAN Xiaoyin;CHEN Peiwen;LIU Zhen;LIU Xiaoxiao(Guangdong Institute for Drug Control,Guangzhou,Guangdong,China 510180)
出处
《中国药业》
2025年第17期80-83,共4页
China Pharmaceuticals
基金
国家药品监督管理局药品监管科学体系建设重点项目[RS2024Z006]
广东省药品监督管理局科技创新项目[2023YDZ10]。
关键词
益气健脾口服液
薄层色谱法
固相萃取
高效液相色谱法
鸡内金
莲子
枸橼酸
Yiqi Jianpi Oral Liquid
TLC
solid phase extraction
HPLC
Galli Gigerii Endothelium Corneum
Nelumbinis Semen
citric acid
