白芷饮片水煎浸膏HPLC指纹图谱及8个特征成分含量测定方法的建立

Establishment of HPLC fingerprinting and content determination methods of eight characteristic components in water-decocted extract of Angelicae Dahuricae Radix

摘要

目的: 采用HPLC技术建立白芷饮片水煎浸膏指纹图谱和8个特征成分的含量测定方法,同时测定14批白芷饮片水煎浸膏指纹图谱及8个特征成分的含量。方法: 采用SinoChrom ODS-BP色谱柱(250 mm×4.6 mm,5 μm),以0.025%磷酸水溶液-乙腈为流动相,程序梯度洗脱,柱温35 ℃,检测波长220 nm,流速分别为1.0 mL·min^－1(指纹图谱)和1.2 mL·min^－1(含量测定)。结果: 白芷饮片水煎浸膏HPLC指纹图谱中含有29个共有峰,鉴定出9个色谱峰成分(花椒毒酚、5-羟基-8甲氧基补骨脂素、水合氧化前胡素、白当归素、花椒毒素、佛手柑内酯、异茴芹内酯、欧前胡素和珊瑚菜素),14批白芷饮片指纹图谱的相似度＞0.980。花椒毒酚、5-羟基-8-甲氧基补骨脂素、水合氧化前胡素、白当归素、花椒毒素、佛手柑内酯、欧前胡素和珊瑚菜素的含量线性范围分别为3.24~162.00、2.86~143.00、3.10~155.00、2.98~149.00、3.12~156.00、3.02~151.0、3.16~158.00和2.30~115.00 μg·mg^－1。14批白芷饮片水煎浸膏中花椒毒酚、5-羟基-8甲氧基补骨脂素、水合氧化前胡素、白当归素、花椒毒素、佛手柑内酯、欧前胡素和珊瑚菜素的含量范围分别为0.14~0.37、0.26~0.39、2.31~3.48、1.09~2.22、0.04~0.26、0.19~0.34、0.03~0.14和0.11~0.23 μg·mg^－1。结论: 该方法具有良好精确性、重复性和稳定性,能较好地反映白芷水煎浸膏的整体成分特征和主要特征成分的含量范围,可用于白芷药材、饮片及其制剂的质量控制。

Abstract

Objective: To establish the HPLC fingerprinting and quantitative method of eight characteristic components in water-decocted extract of Angelicae Dahuricae Radix, and investigate the similarities of 14 batches of Angelicae Dahuricae Radix samples. Methods: SinoChrom ODS-BP column(250 mm×4.6 mm,5 μm)was used for the fingerprinting and quantitative assay. The mobile phase was 0.025% phosphoric acid-acetonitrile under gradient elution mode. The column temperature was 35 ℃, the detection wavelength was 220 nm, the flow rates were 1.0 mL·min^－1 for fingerprinting and 1.2 mL·min^－1 for quantitative assay, respectively. Results: In the HPLC fingerprinting, there were 29 common peaks in 14 batches of Angelicae Dahuricae Radix, and eight characteristic components were identified (xanthotol, 5-hydroxy-8-methoxypsoralen, oxypeucedanin hydrate, byakangelicin, xanthotoxin, bergapten, isoimpinellin, imperatorin, and phellopterin). The fingerprints of the 14 batches of Angelicae Dahuricae Radix were similar and the similarities were greater than 0.980. The linear ranges of xanthotoxol, 5-hydroxy-8-methoxypsoralen, oxypeucedanin hydrate, byakangelicin, xanthotoxin, bergapten, imperatorin, and phellopterin were 3.24~162.00, 2.86~143.00, 3.10~155.00, 2.98~149.00, 3.12~156.00, 3.02~151.0, 3.16~158.00, and 2.30~115.00 μg·mg^－1, respectively. The content ranges of xanthotoxol, 5-hydroxy-8-methoxypsoralen, oxypeucedanin hydrate, byakangelicin, xanthotoxin, bergapten, imperatorin, and phellopterin were 0.14~0.37, 0.26~0.39, 2.31~3.48, 1.09~2.22, 0.04~0.26, 0.19~0.34, 0.03~0.14, and 0.11~0.23 μg·mg^－1, respectively for the 14 batches of Angelicae Dahuricae Radix. Conclusion: The established methods of HPLC fingerprinting and quantitative analysis are reproducible, reliable, and stabile. In the future, these methods can be used for the quality control of original, processed materials and products of Angelicae Dahuricae Radix.

关键词

白芷 / 水煎浸膏 / 指纹图谱 / 含量测定

Key words

Angelicae Dahuricae Radix / water-decocted extract / fingerprinting / content determination

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基金资助

国家中医药管理局高水平重点学科建设资助项目(zyyzdxk-2023311)