HPLC测定枳实导滞丸中枳实所含6种成分及其药材基原分析

HPLC determination of 6 component of Aurantii Fructus Immaturus in Zhishi Daozhi pills and genetic analysis of medicinal materials

目的建立枳实导滞丸中芸香柚皮苷、柚皮苷、橙皮苷、新橙皮苷、水合橙皮内酯、马尔敏的含量测定方法,同时鉴别其中枳实来源。方法采用Waters Symmetry C 18柱(250 mm×4.6 mm,5μm)色谱柱分析,以乙腈(A)-乙酸水(B)为流动相,梯度洗脱,柱温30℃,流速:1.0 mL·min^(-1),检测波长:285 nm、320 nm,进样量10μL。结果6个成分在各自线性范围内均符合要求,相关系数r均≥0.9993;各成分平均回收率范围在98.68%~101.16%,RSD均≤2.5%。12批枳实导滞丸中芸香柚皮苷质量分数在0.37~5.65 mg·g^(-1),柚皮苷在0~12.16 mg·g^(-1),橙皮苷在0~53.90 mg·g^(-1),新橙皮苷在0~18.90 mg·g^(-1),水合橙皮内酯在0~0.23 mg·g^(-1),马尔敏在0~0.13 mg·g^(-1)。12批次枳实导滞丸样品分别呈现与酸橙或甜橙药材一致的黄酮类成分含量情况。香豆素类成分主要存在于酸橙制备的丸剂中且含量偏低。结论该方法简便、准确、可靠,可同时测定枳实导滞丸中6种有效成分的含量并鉴别丸剂中枳实的基原,可为枳实导滞丸质量评价提供依据。

Objective To simultaneous determine 6 constituents in Zhishi Daozhi pills(narirutin,naringin,hesperidin,neohesperidin,meranzin hydrate and marmin)by HPLC,and identify the source of Fructus Aurantii Immaturus.Methods The analysis was performed on a Waters Symmetry C 18 column(250 mm×4.6 mm,5μm),with acetonitrile-0.1%acetic acid solution as the mobile phase for gradient elution.The flow rate was 1.0 mL·min^(-1),the detection wavelength was 285 nm and 320 nm,the column temperature was 30℃,and the injection volume was 10μL.Results All the 6 components met the requirements in their respective linear ranges,and their correlation coefficients(r)were all≥0.9993.The average recovery of each component ranged 98.68%~101.16%,and their RSDs were all less than 2.5%.The contents of narirutin,naringin,hesperidin,neohesperidin,meranzin hydrate and marmin was 0.37~5.56 mg·g^(-1),0~12.16 mg·g^(-1),0~53.90 mg·g^(-1),0~18.90 mg·g^(-1),0~0.23 mg·g^(-1),and 0~0.13 mg·g^(-1),respectively.Totally 12 batches of Zhishi Daozhi pills showed similar content of flavonoids as in Citrus aurantium and Citrus sinensis.Coumarins mainly existed in the pills prepared by Citrus aurantium and their contents was low.Conclusion The method is simple,accurate and reliable,and can be used for the content determination of 6 components simultaneously and identify the source of Fructus Aurantii Immaturus in Zhishi Daozhi pills,which can provide reference for the quality control of Zhishi Daozhi pills.