摘要
目的:建立医疗机构特色中药制剂黄马酊质量标准。方法:采用薄层色谱法(TLC)对黄马酊中的所有药味(黄连、马钱子)进行定性鉴别;采用高效液相色谱法(HPLC),对黄马酊中士的宁、盐酸小檗碱进行含量测定,色谱柱为phenomenex Luna C_(18)色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-乙腈-添加等量0.025 mol·L^(-1)十二烷基硫酸钠的0.1 mol·L^(-1)磷酸二氢钠溶液(50∶25∶25),流速为1.0 mL·min^(-1),检测波长为254 nm,色谱柱柱温为25℃,进样量为10μL。结果:黄连、马钱子的TLC图谱特征斑点清晰,分离度好,且阴性对照无干扰;士的宁、盐酸小檗碱色谱峰保留时间在10 min以内,分离度良好,且空白溶剂无干扰;精密度、重复性、稳定性实验中士的宁、盐酸小檗碱两种化学成分的峰面积相对标准偏差(RSD)均小于3%,黄马酊样品在室温下放置24 h稳定性良好,士的宁、盐酸小檗碱的加样回收率分别为95.58%,97.65%;3批黄马酊中士的宁、盐酸小檗碱的含量分别为0.888±0.077,2.231±0.181 mg·mL^(-1)。结论:本研究建立的方法可操作性强、分析速度快、准确度高且重复性良好,可用于黄马酊的质量控制。
Objective:To establish quality standard of the characteristic traditional Chinese medicine formulation HuangmaTincture.Methods:Qualitative identification of Coptidis Rhizoma and Strychni Semen in the formulation was performed using thin-layer chromatog-raphy(TLC).Quantitative analysis of strychnine and berberine hydrochloride were conducted through high-performance liquid chromatog-raphy(HPLC),employing a Phenomenex Luna C_(18) column(250×4.6 mm,5μm).The mobile phase consisted of methanol-acetonitrile-0.1 mol·L^(-1)sodium dihydrogen phosphate solution containing the same volume of 0.025 mol·L^(-1)sodium dodecyl sulfate solution(50∶25∶25),with a flow rate set at 1.0 mL·min^(-1).Detection was carried out at a wavelength of 254 nm with column temperature at 25℃and 10μL sam-ples injected.Results:The TLC profiles of Coptidis Rhizoma and Strychni Semen showed clear and well-separated spots with no interfer-ence from the negative controls.The HPLC peaks for strychnine and berberine hydrochloride were retained within 10 minutes,demonstrating good separation with no interference from the blank solvent.Precision,repeatability,and stability tests revealed relative standard deviations(RSD)of peak areas for both chemical components to be less than 3%.The sample solutions were stable at room temperature for 24 hours,with spike recoveries of strychnine and berberine hydrochloride at 95.58%and 97.65%,respectively.The mean values of the contents of s strychnine and berberine hydrochloride in 3 batches of Huangma Tincture were 0.888±0.077 mg·mL^(-1)and 2.231±0.181 mg·mL^(-1),respec-tively.Conclusion:The methods developed in this study are simple,time-efficient and accurate,making them suitable for quality control of Huangma Tincture.
作者
邱菁
李杰
冷静
QIU Jing;LI Jie;LENG Jing(Preparationcenter,Chongqing Hospital of Traditional Chinese Medicine,Chongqing Jiangbei 400021,China)
出处
《中药与临床》
2025年第6期13-17,共5页
Pharmacy and Clinics of Chinese Materia Medica
基金
重庆市科研机构绩效激励引导专项项目(cstc2021jxjl 10001,cstc2018jxjl 130029)。
