中国临床药理学杂志

用UPLC-MS/MS法同时测定活血消肿胶囊中8种成分的含量

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王甜甜 ¹ , 付冉 ² , 李德强 ¹ , 于静 ² , 卓婷婷 ¹ , 白晓梅 ¹ , 代鹏 ¹ , 周春华 ²

中国临床药理学杂志 | 研究方法 2025,41(22): 3228-3233

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中国临床药理学杂志 |研究方法 2025 , 41 (22) : 3228 -3233

用UPLC-MS/MS法同时测定活血消肿胶囊中8种成分的含量

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王甜甜¹, 付冉², 李德强¹, 于静², 卓婷婷¹, 白晓梅¹, 代鹏¹, 周春华²

作者信息

^1.河北医科大学第二医院鹿泉院区药学部，河北石家庄 050000

^2.河北医科大学第一医院临床药学部，河北石家庄 050000

通讯作者:

周春华，教授，博士生导师 Tel: （0311）87156675 E-mail: zhouchunhua@hebcm.edu.cn

作者简介:

王甜甜（1990-），女，主管药师，主要从事临床药学相关研究

Simultaneous determination of eight constituents in Huoxuexiaozhong capsules by UPLC-MS/MS

Tian-tian WANG¹, Ran FU², De-qiang LI¹, Jing YU², Ting-ting ZHUO¹, Xiao-mei BAI¹, Peng DAI¹, Chun-hua ZHOU²

Affiliations

^1.Department of Pharmacy, The Second Hospital of Hebei Medical University, Shijiazhuang 050000, Hebei Province, China

^2.Department of Pharmacy, The First Hospital of Hebei Medical University, Shijiazhuang 050000, Hebei Province, China

出版时间: 2025-11-28 doi: 10.13699/j.cnki.1001-6821.2025.22.012

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摘要

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目的

建立一种超高效液相色谱串联三重四极杆质谱（UPLC-MS/MS）法同时测定活血消肿胶囊中胆酸、欧前胡素、槲皮素、异槲皮苷、阿魏酸、绿原酸、芦丁、隐绿原酸的含量。

方法

采用UPLC-MS/MS法测定活血消肿胶囊中8种成分的含量。色谱条件：色谱柱为Agilent Poroshell 120 EC-C₁₈（2.1×150 mm，1.9 μm），流动相为乙腈（A）-0.1%甲酸水（B），流速为0.3 mL·min^-1，柱温为35 ℃；质谱条件：电喷雾离子源，以多反应监测（MRM）模式进行正负离子切换扫描。离子源电压分设5.5 kV和-4.5 kV，离子源温度550 ℃，GS1 344.74 kPa，GS2 344.74 kPa，CUR 241.32 kPa。考察该方法的专属性、标准曲线与定量下限、精密度与回收率和稳定性。

结果

胆酸、槲皮素、异槲皮苷、阿魏酸、绿原酸、隐绿原酸、芦丁和欧前胡素分别在（0.26~25.70）、（0.03~1.68）、（0.03~1.51）、（0.03~1.47）、（0.40~10.34）、（0.56~27.05）、（0.03~1.37）、（2.50~759.65）μ·mL^-1的浓度范围内线性关系良好（R²≥0.991 1）；对照品和供试品的峰面积相对标准偏差（RSD）分别≤2.44%和≤2.87%，各成分的加样回收率在96.54%~107.86%之间，RSD在0.47%~5.41%，精密度和准确度良好；稳定性相对标准偏差≤2.77%。

结论

本研究建立了同时测定活血消肿胶囊中8种成分浓度的UPLC-MS/MS方法，该法灵敏度高、特异性、稳定性强，可为活血消肿胶囊质量控制提供参考。

关键词

活血消肿胶囊 / 化学成分 / 超高效液相色谱串联三重四极杆质谱 / 含量测定

Abstract

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Objective

To establish an ultra-high performance liquid chromatography-tandem mass spectrometry method (UPLC-MS/MS) for the determination of the contents of cholic acid, imperatorin, quercetin, isoquercetin, ferulic acid, chlorogenic acid, rutin, and cryptochlorogenic acid in the Huoxuexiaozhong capsule.

Methods

The analysis was performed by UPLC-MS/MS. Chromatographic conditions: separation was achieved on an Agilent Poroshell 120 EC-C₁₈ column (2.1×150 mm, 1.9 μm). The mobile phase consisted of acetonitrile (A) and 0.1% formic acid in water (B) with gradient elution, at a flow rate of 0.3 mL·min^-1 and a column temperature of 35 ℃. Mass spectrometry conditions: multiple reaction monitoring (MRM) with positive/negative ion switching mode was used electrospray ionization source. The ion source voltage was set at +5.5 kV and -4.5 kV, with the ion source temperature maintained at 550 ℃. The gas settings were as follows: GS1 344.74 kPa, GS2 344.74 kPa, and CUR 241.32 kPa. The specificity, standard curves and limits of detection and quantification, precision and recovery, and stability were investigated.

Results

The analytical method demonstrated good linearities for cholic acid, quercetin, isoquercitrin, ferulic acid, chlorogenic acid, cryptochlorogenic acid, rutin and imperatorin over the concentration ranges of (0.26-25.70), (0.03-1.68), (0.03-1.51), (0.03-1.47), (0.40-10.34), (0.56-27.05), (0.03-1.37), and (2.50-759.65) μg·mL^-1, respectively (R² ≥ 0.9911). The relative standard deviations (RSD) of peak areas for reference standards and test samples were ≤ 2.44% and ≤ 2.87%, respectively. Recoveries for all components ranged from 96.54% to 107.86%, with RSD values between 0.47% and 5.41%, indicating good precision and accuracy. The stability of the method showed an RSD of ≤ 2.77%.

Conclusion

The UPLC-MS/MS method was established to determine the concentration of eight components in Huoxuexiaozhong capsule simultaneously. This method has high sensitivity, specificity and stability, which can be used as a reliable reference for the quality control of the capsule.

Key words

Huoxuexiaozhong capsule / chemical composition / UPLC-MS/MS / content determination

引用本文

王甜甜, 付冉, 李德强, 于静, 卓婷婷, 白晓梅, 代鹏, 周春华. 用UPLC-MS/MS法同时测定活血消肿胶囊中8种成分的含量. 中国临床药理学杂志, 2025 , 41 (22) : 3228 -3233 . DOI: 10.13699/j.cnki.1001-6821.2025.22.012

Tian-tian WANG, Ran FU, De-qiang LI, Jing YU, Ting-ting ZHUO, Xiao-mei BAI, Peng DAI, Chun-hua ZHOU. Simultaneous determination of eight constituents in Huoxuexiaozhong capsules by UPLC-MS/MS[J]. Chinese Journal of Clinical Pharmacology, 2025 , 41 (22) : 3228 -3233 . DOI: 10.13699/j.cnki.1001-6821.2025.22.012

基金

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河北省中医药管理局科研计划重点基金资助项目(NoZ2022014)

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2025年第41卷第22期

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文章信息

doi: 10.13699/j.cnki.1001-6821.2025.22.012

接收时间：2025-08-04
首发时间：2026-08-05
出版时间：2025-11-28

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收稿日期：2025-08-04

基金

河北省中医药管理局科研计划重点基金资助项目(NoZ2022014)

作者信息

^1.河北医科大学第二医院鹿泉院区药学部，河北石家庄 050000

^2.河北医科大学第一医院临床药学部，河北石家庄 050000

通讯作者:

周春华，教授，博士生导师 Tel: （0311）87156675 E-mail: zhouchunhua@hebcm.edu.cn

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2种不同金属材料的力学参数

科 Family	属数 Number of genus	种数 Number of species	占总种数比例 Percentage of total species (%)	属 Genus	种数 Number of species	占总种数比例 Percentage of total species (%)
鹅膏菌科Amanitaceae	2	11	5.26	鹅膏菌属 Amanita	10	4.78
小菇科 Mycenaceae	2	12	5.74	丝盖伞属 Inocybe	5	2.39
多孔菌科 Polyporaceae	8	14	6.70	蜡蘑属 Laccaria	5	2.39
红菇科 Russulaceae	3	23	11.00	小皮伞属 Marasmius	6	2.87
				小菇属 Mycena	11	5.26
				光柄菇属 Pluteus	5	2.39
				红菇属 Russula	17	8.13
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