Page 69 - 《中国药房》2022年11期

当归补血丸指纹图谱及3种指标成分含量测定方法的建立 Δ

范佳儿 ，刘银榕 ，晁 志 ，田恩伟 1，2，3 # （1.南方医科大学中医药学院，广州 510515；2.广东省中药制剂重点实
1
1＊
1
验室，广州 510515；3.广东省中药制剂技术工程实验室，广州 510515）
中图分类号 R917 文献标志码 A 文章编号 1001-0408（2022）11-1343-06
DOI 10.6039/j.issn.1001-0408.2022.11.11

摘 要 目的 建立当归补血丸的指纹图谱以及3种指标性成分（阿魏酸、毛蕊异黄酮葡萄糖苷、黄芪甲苷）的含量测定方法。方
法 以来自 2 个厂家的 15 批当归补血丸为样品，采用高效液相色谱（HPLC）法进行分析。色谱柱为 Hypersil ODS2 C18；柱温为
25 ℃；流动相为乙腈-0.2％甲酸溶液（梯度洗脱）；流速为1.0 mL/min；进样量为20 μL；检测器为紫外检测器[检测波长分别为250
nm（毛蕊异黄酮葡萄糖苷）、323 nm（阿魏酸）]和蒸发光散射检测器（黄芪甲苷）。通过《中药色谱指纹图谱相似度评价系统（2012
版）》建立15批当归补血丸的HPLC指纹图谱并进行相似度评价，通过与对照品图谱及对照药材图谱比对进行色谱峰的指认和归
属，并测定其中阿魏酸、毛蕊异黄酮葡萄糖苷、黄芪甲苷的含量。结果 15 批样品指纹图谱中有 33 个共有峰，相似度均不低于
0.893，并指认出13号峰为阿魏酸、15号峰为毛蕊异黄酮葡萄糖苷；通过与对照药材色谱图进行比对，发现1～3、7、8、10、12、13（阿
魏酸）、17～19、27～29、32、33号峰归属于当归，14、15（毛蕊异黄酮葡萄糖苷）、20～23、25号峰归属于黄芪。含量测定方法学考察
结果均符合相关要求，15批样品中阿魏酸、毛蕊异黄酮葡萄糖苷、黄芪甲苷的平均含量分别为0.050 1、0.402 6、0.913 4 mg/g。结论 本
研究建立了当归补血丸的HPLC指纹图谱及3种指标成分的HPLC定量分析方法，所建方法准确可靠、重复性好。
关键词 当归补血丸；指纹图谱；阿魏酸；毛蕊异黄酮葡萄糖苷；黄芪甲苷；含量测定；质量控制

Establishment of the fingerprints for Danggui buxue pills and the method for the content determination of
three indicative constituents
1
1
FAN Jia’er ，LIU Yinrong ，CHAO Zhi ，TIAN Enwei 1，2，3 （1. School of Traditional Chinese Medicine，Southern
1
Medical University，Guangzhou 510515，China；2. Guangdong Province Key Laboratory of TCM，Guangzhou
510515，China；3. Guangdong Laboratory of TCM Preparation Technology Engineering，Guangzhou 510515，
China）

ABSTRACT OBJECTIVE To establish the fingerprints of Danggui buxue pills and the method for the content determination of
three indicative constituents （ferulic acid，calycosin 7-O-β-D-glucoside and astragaloside Ⅳ）. METHODS Fifteen batches of
Danggui buxue pills from two manufacturers were analyzed by high performance liquid chromatography （HPLC）. The
determination was performed on a Hypersil ODS2 C18 column with mobile phase consisted of acetonitrile-0.2％ formic acid
（gradient elution）at the flow rate of 1.0 mL/min. The column temperature was set at 25 ℃，and the sample size was 20 μL. UV
detector [detection wavelengths were 250 nm （calycosin 7-O-β-D-glucoside），323 nm （ferulic acid）] and evaporative light
scattering detector（astragaloside Ⅳ）were selected as detectors. HPLC fingerprints of 15 batches of Danggui buxue pills were
established with Similarity Evaluation System of TCM Chromatographic Fingerprint （2012 edition）. The chromatographic peaks
were identified and assigned by comparing with the chromatogram of the reference substance and reference medicinal material；the
contents of ferulic acid，calycosin 7-O-β-D-glucoside and astragaloside Ⅳ were also determined. RESULTS There were 33
common peaks in the fingerprints of 15 batches of samples with the similarities not lower than 0.893. Ferulic acid and calycosin
7-O-β-D-glucoside were identified as peak 13 and 15，respectively. Compared with the chromatogram of reference medicinal
material，it could be found that peaks 1-3，7，8，10，12，13（ferulic acid），17-19，27-29，32 and 33 belonged to Angelica
sinensis，and peak 14，15（calycosin 7-O-β-D-glucoside），20-23，25 belonged to Astragalus membranaceus. The methodology of
content determination met the requirements. The mean contents of ferulic acid，calycosin 7-O-β-D-glucoside and astragaloside Ⅳ in
15 batches of samples were 0.050 1，0.402 6，0.913 4 mg/g. CONCLUSIONS In this study，HPLC fingerprints of Danggui buxue
pills and the method of HPLC quantitative analysis for three
Δ 基金项目：广东省科技计划项目（No.2016A020226029）；广州
市科技计划项目（No.2022-01-01-11-3028-0066）；2021年南方医科大学 indicative constituents are established. Established methods are
“科研启蒙计划项目” accurate，reliable and repeatable.
＊本科生。研究方向：中药鉴定与质量控制。E-mail：2983997864 KEYWORDS Danggui buxue pills； fingerprints； ferulic
@qq.com acid；calycosin 7-O-β-D-glucoside；astragaloside Ⅳ ；content
# 通信作者：副教授，硕士生导师，博士。研究方向：中药资源与 determination；quality control
质量控制。E-mail：tianenwei@126.com

中国药房 2022年第33卷第11期 China Pharmacy 2022 Vol. 33 No. 11 ·1343 ·