Page 63 - 《中国药房》2023年9期

HPLC指纹图谱结合一测多评法控制马齿苋药材质量 Δ

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王佳佳 ，李 希 1， 2 # ，冯建安 ，楼冠华 ，陈诗韵 ，黄 嫣 ，皮雪莲 ，刘 畅 ，李 颖（1.成都中医药大学药学
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院，成都 611137；2.四川省中医药科学院中医研究所，成都 610031）
中图分类号 R917；R284.1 文献标志码 A 文章编号 1001-0408（2023）09-1081-05
DOI 10.6039/j.issn.1001-0408.2023.09.11
摘 要 目的 建立马齿苋药材的高效液相色谱（HPLC）指纹图谱，同时建立一测多评法测定该药材中咖啡酸、阿魏酸、染料木苷、
槲皮素的含量，为该药材的质量控制提供参考依据。方法 色谱柱为Eclipse XDB-C18，流动相为甲醇-0.2%磷酸溶液（梯度洗脱），
柱温为25 ℃ ，流速为1.0 mL/min，检测波长为360 nm，进样量为10 μL，以上述色谱条件建立马齿苋药材的HPLC指纹图谱；对15
批药材样品进行聚类分析和主成分分析；以咖啡酸作为内标物，使用一测多评法计算其他3种成分的相对校正因子，再根据相对
校正因子计算成分含量，并与外标法结果进行比较。结果 15批马齿苋药材样品的HPLC指纹图谱中有17个共有峰被标定，4种
成分（咖啡酸、阿魏酸、染料木苷、槲皮素）被指认；15批样品的相似度均大于0.890。聚类分析结果显示，样品S1～S10聚为一类，
S11～S15聚为一类；主成分分析结果显示，前2个主成分的累计贡献率为92.502%，分类结果与聚类分析结果一致。咖啡酸、阿魏
酸、染料木苷和槲皮素检测质量浓度的线性范围分别为0.003 1～0.157 1、0.003 6～0.181 7、0.008 5～0.425 6、0.000 4～0.021 8 mg/mL
（R ≥0.999 7）；精密度、重复性、稳定性（24 h）、加样回收率试验结果均符合《中国药典》要求。一测多评法计算得到阿魏酸、染料木
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苷、槲皮素的平均相对校正因子分别为1.534、5.302、0.174，该方法与外标法所测的成分含量无显著差异。结论 所建立的HPLC
指纹图谱结合一测多评的方法，可用于马齿苋药材中多指标成分的质量控制。产地对马齿苋药材质量有一定影响，四川所产马齿
苋药材质量略优于安徽和河北所产药材。
关键词 马齿苋；质量控制；高效液相色谱法；指纹图谱；一测多评法；咖啡酸；阿魏酸；染料木苷；槲皮素

Quality control of Portulaca oleracea by HPLC fingerprint combined with quantitative analysis of multi-
components by single-marker
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WANG Jiajia ，LI Xi ，FENG Jian’an ，LOU Guanhua ，CHEN Shiyun ，HUANG Yan ，PI Xuelian ，LIU Chang ，
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LI Ying（1. School of Pharmacy， Chengdu University of Chinese Medicine，Chengdu 611137，China；2. Institute
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of Traditional Chinese Medicine， Sichuan Academy of Chinese Medicine Sciences， Chengdu 610031， China）
ABSTRACT OBJECTIVE To establish HPLC fingerprint of Portulaca oleracea， establish quantitative analysis of multi-
components by single-marker （QAMS） method for the content determination of caffeic acid， ferulic acid， genistin and quercetin，
and provide reference for quality control of the medicine. METHODS The determination was performed on Eclipse XDB-C18
column with mobile phase consisted of methanol-0.2% phosphoric acid solution （gradient elution） at the flow rate of 1.0 mL/min.
The column temperature was 25 °C， and detection wavelength was set at 360 nm. The sample size was 10 μL. HPLC fingerprint of
P. oleracea was established according to the above chromatographic conditions. Cluster analysis （CA） and principal component
analysis （PCA） were performed for 15 batches of specimens. Using caffeic acid as internal standard， relative correction factors of
other three components were calculated by QAMS， and then the component content was calculated on the basis of relative
correction factors， which was compared with the external standard method. RESULTS HPLC fingerprints of 15 batches of P.
oleracea were calibrated with a total of 17 common peaks， and 4 components （caffeic acid， ferulic acid， genistin， quercetin） were
identified； the similarities of 15 batches of samples were greater than 0.890. The results of CA showed that S1-S10 were clustered
into one category， and S11-S15 were clustered into one category. The results of PCA revealed that the accumulative contribution
rate of the two main components was 92.502%， and the classification results were basically consistent with CA. The linear range of
caffeic acid， ferulic acid， genistin and quercetin were 0.003 1-0.157 1， 0.003 6-0.181 7， 0.008 5-0.425 6，0.000 4-0.021 8 mg/mL
（R ≥0.999 7）； the results of precision， repeatability， stability （24 h） and recovery tests all complied with the requirements of
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Chinese Pharmacopoeia. The relative correction factors of
Δ 基金项目 四川省中医药管理局科学技术研究专项课题（No.
ferulic acid， genistin and quercetin calculated by QAMS were
2021MS032）
1.534， 5.302 and 0.174； there was no significant difference in
＊第一作者 硕士研究生。研究方向：中药新制剂、新剂型、新技术
应用。E-mail：1598470388@qq.com the contents of components measured between this method and
# 通信作者 研究员，主任中药师，硕士生导师，硕士。研究方向： the external standard method. CONCLUSIONS The
中药新制剂、新剂型、新技术应用。E-mail：1836820767@qq.com established HPLC fingerprint combined with QAMS can be

中国药房 2023年第34卷第9期 China Pharmacy 2023 Vol. 34 No. 9 · 1081 ·