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1.陕西省中医药研究院(陕西省中医医院)中药研究所,西安;710003
2.西北大学生命科学学院,西安 710069
3.西安中医脑病医院制剂中心,西安 710032
4.西安市中药制剂工程技术研究中心,西安 710032
研究实习员,硕士。研究方向:中药质量控制与分析。E-mail:zhangxy9605@163.com
副研究员,博士。研究方向:中药药效物质基础。 E-mail:liuyang311111@163.com
收稿:2025-06-06,
修回:2025-08-25,
录用:2025-08-25,
纸质出版:2025-10-15
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张笑颜,丁凯茹,张红,等.麝川脑立通颗粒的HPLC指纹图谱及一测多评含量测定方法研究[J].中国药房,2025,36(19):2409-2414.
ZHANG Xiaoyan,DING Kairu,ZHANG Hong,et al.Study on HPLC fingerprint and quantitative analysis of multi-components by single-marker content determination method for Shechuan naolitong granules[J].ZHONGGUO YAOFANG,2025,36(19):2409-2414.
张笑颜,丁凯茹,张红,等.麝川脑立通颗粒的HPLC指纹图谱及一测多评含量测定方法研究[J].中国药房,2025,36(19):2409-2414. DOI: 10.6039/j.issn.1001-0408.2025.19.09.
ZHANG Xiaoyan,DING Kairu,ZHANG Hong,et al.Study on HPLC fingerprint and quantitative analysis of multi-components by single-marker content determination method for Shechuan naolitong granules[J].ZHONGGUO YAOFANG,2025,36(19):2409-2414. DOI: 10.6039/j.issn.1001-0408.2025.19.09.
目的
2
为优化和提升麝川脑立通颗粒的质量标准提供参考依据。
方法
2
以15批麝川脑立通颗粒为样品,通过《中药色谱指纹图谱相似度评价系统(2012版)》建立其高效液相色谱(HPLC)指纹图谱,进行相似度评价和共有峰指认,并通过正交偏最小二乘-判别分析(OPLS-DA)对其进行质量差异评价,筛选质量差异性成分。以丹酚酸B(SAB)为内参物,建立京尼平苷酸(GA)、绿原酸(CA)、王不留行黄酮苷(VA)、阿魏酸(FA)、洋川芎内酯I(SI)的一测多评法,并与外标法测定结果进行比较。
结果
2
在15批样品指纹图谱中共标定出13个共有峰,图谱相似度均大于0.96;指认出其中7个色谱峰,分别为GA(峰3)、CA(峰6)、VA(峰8)、FA(峰9)、SI(峰11)、SAB(峰12)、TA(峰13)。OPLS-DA结果表明,15批样品的质量差异性成分为峰5、11(SI)、12(SAB)。以SAB为内参物,计算得GA、CA、VA、FA、SI的相对校正因子分别为1.058 4、0.594 3、0.643 3、0.342 7、0.262 8,一测多评法测得的15批样品中GA、
CA、VA、FA、SI和SAB的平均含量分别为0.155 0、0.085 4、0.140 3、0.071 8、0.072 7、1.276 3 mg/g,与外标法测定结果差异无统计学意义(
P
>0.05)。
结论
2
所建立的HPLC指纹图谱和一测多评法操作简便且高效、经济,可为麝川脑立通颗粒质量控制与深入开发提供参考。
OBJECTIVE
2
To provide a reference for optimizing and promoting the quality standards of Shechuan naolitong granules.
METHODS
2
Fifteen batches of Shechuan naolitong granules were used as samples to establish HPLC fingerprints using the
Similarity Evaluation System for Chromatographic Fingerprint of Traditional Chinese Medicine
(
2012 edition
). Similarity evaluation and common peak identification were performed, and orthogonal partial least squares discriminant analysis (OPLS-DA) was used to assess quality differences among different batches and to screen quality differential components. Using salvianolic acid B(SAB) as the internal reference, quantitative analysis of multi-components by single-marker (QAMS) was developed to simultaneously determine geniposidic acid (GA), chlorogenic acid (CA), vaccarin (VA), ferulic acid (FA) and senkyunolide I (SI). The results were compared with those obtained by the external standard method.
RESULTS
2
A total of 13 common peaks were identified in the HPLC fingerprints of 15 batches of samples, and the similarities of the spectra were all above 0.96. Seven chromatographic peaks were identified as GA (peak 3), CA (peak 6), VA (peak 8), FA (peak 9), SI (peak 11), SAB(peak 12) and TA(peak 13). OPLS-DA indicated that the differential quality markers among 15 batches were peaks 5, 11 (SI), and 12 (SAB). Using SAB as the internal reference, the relative correction factors for GA, CA, VA, FA and SI were calculated as 1.058 4, 0.594 3, 0.643 3, 0.342 7 and 0.262 8, respectively. The mean content of GA, CA, VA, FA, SI and SAB across the 15 batches of samples were 0.155 0, 0.085 4, 0.140 3, 0.071 8
, 0.072 7, 1.276 3 mg/g, respectively, showing no significant difference compared with the ESM (
P
>0.05).
CONCLUSIONS
2
The established HPLC fingerprint and QAMS are simple, efficient and economical, providing a reference for the quality control and further development of Shechuan naolitong granules.
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