摘要
目的 为左归饮的质量控制提供依据.方法 采用高效液相色谱(HPLC)法建立 15 批左归饮样品的指纹图谱,色谱柱为Agilent 5 HC-C18 柱(250 mm×4.6 mm,5 μm),流动相为 0.2%甲酸水溶液-乙腈(梯度洗脱),流速为 1.0 mL/min,检测波长为250 nm,柱温为 30℃,进样量为 20 μL.采用中药色谱指纹图谱相似度评价系统(2012.1307023 版)进行相似度评价,确定共有峰及指认成分,并测定其含量.结果 15 批样品指纹图谱与对照指纹图谱的相似度均在 0.975～0.999 之间.标定共有峰 33 个,指认出其中5 个,分别为 5-羟甲基糠醛、莫诺苷、马钱苷、甘草苷、甘草酸.5 种成分质量浓度分别在 0.017～0.266 mg/mL、0.049～0.784 mg/mL、0.034～0.539 mg/mL、0.016～0.250 mg/mL、0.009～0.150 mg/mL范围内与峰面积线性关系良好(R2>0.9990,n=5);精密度、稳定性、重复性试验结果的 RSD 均小于 3.0%;平均加样回收率分别为 101.40%,98.72%,98.00%,101.53%,99.13%,RSD分别为 2.06%,2.09%,1.65%,1.56%,0.40%(n=6);样品含量分别为 49.838～140.933 μg/g、131.060～340.103 μg/g、68.081～178.313 μg/g、12.108～47.326 μg/g、1.190～55.483 μg/g.结论 所建立的方法可用于左归饮HPLC指纹图谱的建立及其中 5 个成分的含量测定,可更全面地为左归饮的质量评价提供依据.
Abstract
Objective To provide a basis for the quality control of Zuogui Drink.Methods Fingerprint of 15 batches of Zuogui Drink samples was established by the high-performance liquid chromatography(HPLC)method.The chromatographic column was the Agilent 5 HC-C18 column(250 mm×4.6 mm,5 μm),the mobile phase was 0.2%formic acid aqueous solution-acetonitrile(gradient elution),the flow rate was 1.0 mL/min,the detection wavelength was 250 nm,the column temperature was 30℃,and the injection volume was 20 μL.The Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine(Version 2012.1307023)was used for similarity evaluation,the common peaks were marked,the components were identified,and the contents were determined.Results The similarity between the fingerprint of 15 batches of samples and the reference fingerprint was in the range of 0.975-0.999.A total of 33 common peaks were marked,and five of them were identified,namely 5-hydroxymethylfurfural(5-HMF),morroniside,loganin,liquiritin and glycyrrhizic acid.The linear ranges of the above five components were 0.017-0.266 mg/mL,0.049-0.784 mg/mL,0.034-0.539 mg/mL,0.016-0.250 mg/mL,and 0.009-0.150 mg/mL(R2>0.9990,n=5)respectively.The RSDs of precision,stability and repeatability tests were all lower than 3.0%.The average recovery rates of the above five components were 101.40%,98.72%,98.00%,101.53%,99.13%,with RSDs of 2.06%,2.09%,1.65%,1.56%,0.40%(n=6)respectively.The contents of 5-HMF,morroniside,loganin,liquiritin and glycyrrhizic acid in samples were in the range of 49.838-140.933 μg/g,131.060-340.103 μg/g,68.081-178.313 μg/g,12.108-47.326 μg/g,and 1.190-55.483 μg/g,respectively.Conclusion The established method can be used for the establishment of HPLC fingerprint of Zuogui Drink and the contents determination of the five components,which can provide a basis for the comprehensive quality evaluation of Zuogui Drink.
基金项目
国家自然科学基金(82204805)
安徽中医药大学临床科研项目(2021efylc03)
安徽省名中药师工作室项目([皖中医药发展秘[2023]23号])
国家科技期刊平台
NSTL
万方数据