Ingredient Analysis

Simultaneous determination of fourteen active components in Qiyu Sanlong decoction by UPLC-QQQ MS/MS*

  • WEI Zi-qi ,
  • YANG Rui ,
  • LI Lan-ying ,
  • JIANG Yu-ge ,
  • YANG Mo ,
  • ZHOU An ,
  • LI Ze-geng ,
  • WU Huan
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  • 1. College of Pharmacy, Anhui University of Chinese Medicine, Hefei 230012, China;
    2. Key Laboratory of Xin'an Medicine,Ministry of Education, Hefei 230012, China;
    3. Anhui Province Key Laboratory of the Application and Transformation of Traditional Chinese Medicine in the Prevention and Treatment of Major Pulmonary Diseases, Hefei 230031, China

Online published: 2025-10-13

Abstract

Objective: To establish an ultra-performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QQQ MS/MS) method for the simultaneous determination of 14 active components in Qiyu Sanlong decoction, including L-argnine, monotropein, deacetyl asperulosidic acid, rutin, peimisine, calycosin-7-O-β-D-glucoside, caffeic acid, solasonine, solamargine, p-coumaric acid, ferulic acid, calycosin, astragaloside Ⅳ and astragaloside Ⅰ. Methods: The chromatographic separation experiment was performed on an ACQUITY UPLC BEH C18 column(2.1 mm×100 mm, 1.7 μm), with gradient elution of 0.1% formic acid aqueous solution (A)-acetonitrile (B) as mobile phase at the flow rate of 0.2 mL · min-1, injection volume of 5 μL, and column temperature of 35 ℃. The ion source was an electrospray ionization source (ESI), the scanning mode was simultaneous scanning of positive and negative ions, and the monitoring mode was multiple reaction monitoring. Results: The 14 active components revealed good linearity within their respective ranges (r>0.995 0), RSDs of precision and repeatability were below 2%, RSDs of stability were below 3%, and the average recoveries ranged from 88.4% to 108.5% with the RSDs ranging from 0.020% to 3.6%. The content ranges of the aforementioned 14 components in 10 batches of self-prepared Qiyu Sanlong decoction were as follows (in μg · g-1): 667.28-785.78, 165.72-197.27, 196.32-275.60, 17.60-26.52, 4.68-10.75, 279.12-388.05, 26.00-47.57, 385.52-442.77, 288.00-358.82, 629.88-839.02, 86.67-125.83, 51.58-65.83, 25.50-37.53, and 55.50-76.13. Conclusion: The UPLC-QQQ MS/MS method established in this study is rapid, accurate, sensitive and repeatable, which can provide a reference for the quality control of Qiyu Sanglong decoction.

Cite this article

WEI Zi-qi , YANG Rui , LI Lan-ying , JIANG Yu-ge , YANG Mo , ZHOU An , LI Ze-geng , WU Huan . Simultaneous determination of fourteen active components in Qiyu Sanlong decoction by UPLC-QQQ MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2025 , 45(5) : 779 -795 . DOI: 10.16155/j.0254-1793.2024-1216

References

[1] 童佳兵,高雅婷,范春雷,等.芪玉三龙汤治疗中晚期非小细胞肺癌临床观察[J].新中医,2018,50(4):146
TONG JB,GAO YT,FAN CL,et al.Clinical observation of Qiyu Sanlong decoction for non-small cell lung cancer in moderate and advanced stages[J].New J Tradit Chin Med,2018,50(4):146
[2] 高雅婷,王心恒,王小乐,等.芪玉三龙汤调节mTOR/Beclin1/LC3信号轴相关分子的表达诱导肺癌A549细胞自噬[J].中国实验方剂学杂志,2021,27(1):98
GAO YT,WANG XH,WANG XL,et al.Effect of Qiyu Sanlong decoction in inducing autophagy of A549 cells by regulating molecular expression related to signal axis of mTOR-Beclin1-LC3[J].Chin J Exp Tradit Med Form,2021,27(1):98
[3] 刘桐,王小乐,高雅婷,等.芪玉三龙汤药物血清对肺癌A549细胞增殖及凋亡的影响[J].中国中医药信息杂志,2022,29(1):85
LIU T,WANG XL,GAO YT,et al.Effects of Qiyu Sanlong decoction containing serum on proliferation and apoptosis of lung cancer A549 cells[J].Chin J Inf Tradit Chin Med,2022,29(1):85
[4] 焦安男,吴欢,朱洁,等.芪玉三龙汤通过PD-1信号通路增强Th1免疫反应抑制肺癌转移[J].安徽医科大学学报,2022,57(11):1718
JIAO AN,WU H,ZHU J,et al.Qiyu Sanlong decoction enhances Th1 immune response through PD-1 signaling pathway and inhibits metastasis of lung cancer[J].Acta Universitatis Medicinalis Anhui,2022,57(11):1718
[5] 黄梦文,吴欢,于伟,等.超高效液相色谱-四极杆-飞行时间质谱法快速辨识芪玉三龙汤化学成分[J].色谱,2021,39(7):730
HUANG MW,WU H,YU W,et al.Rapid identification of chemical components in Qiyu Sanlong decoction by ultra high performance liquid chromatography-quadrupole time-of-flight mass spectrometry[J].Chin J Chromatogr,2021,39(7):730
[6] ZHENG T,ZHAO Y,LI RJ,et al.The dynamic metabolic profile of Qiyu Sanlong decoction in rat urine using UPLC-QTOF-MSE coupled with a post-targeted screening strategy[J].J Pharm Anal,2022,12(5):755
[7] ZHAO Y,CHEN Y,LI RJ,et al.An ultra-performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry method based on a four-step analysis strategy to investigate metabolites of Qiyu Sanlong decoction in rat plasma[J].Rapid Commun Mass Spectrom,2023,37(1):e9419
[8] FU XJ,ZHENG T,LI ZG,et al.Metabolic profiling of Qiyu Sanlong decoction in rat feces by ultraperformance liquid chromatography-quadrupole time-of-flight mass spectrometry combined with a post-targeted screening strategy[J].Biomed Chromatogr,2023,37(12):e5748
[9] HUANG MW,LI RJ,YANG M,et al.Discovering the potential active ingredients of Qiyu Sanlong decoction for anti-oxidation,inhibition of non-small cell lung cancer based on the spectrum-effect relationship combined with chemometric methods[J].Front Pharmacol,2022,13:989139.doi:10.3389/fphar.2022.989139
[10] 赵越. 基于内外源性代谢物关联性分析的芪玉三龙汤抑制肺腺癌药效物质基础研究[D].合肥:安徽中医药大学,2023
ZHAO Y.Study on the Pharmacodynamic Substances of Qiyu Sanlong Decoction in Inhibiting Lung Adenocarcinoma Based on the Correlation Analysis of Endogenous and Exogenous Metabolites[D].Hefei:Anhui University of Chinese Medicine,2023
[11] 张佳颖,尹艺,徐倩倩,等.UPLC-MS/MS方法同时测定左金丸中23个成分的含量[J].药物分析杂志,2023,43(7):1110
ZHANG JY,YIN Y,XU QQ,et al.Simultaneous determination of content of 23 components in Zuojin pills based on UPLC-MS/MS[J].Chin J Pharm Anal,2023,43(7):1110
[12] 李均艳,李舒琪,刘辉,等.UPLC-MS/MS法同时测定排石合剂中10个特征成分含量[J].药物分析杂志,2023,43(12):2090
LI JY,LI SQ,LIU H,et al.Simultaneous determination of 10 representative components in Paishi mixture by UPLC-MS/MS[J].Chin J Pharm Anal,2023,43(12):2090
[13] LIU F,NONG XJ,QU WH,et al.Pharmacokinetics and tissue distribution of 12 major active components in normal and chronic gastritis rats after oral administration of Weikangling capsules[J].J Ethnopharmacol,2023,316:116722.doi:10.1016/j.jep.2023.116722
[14] XU F,CUI WQ,WEI Y,et al.Astragaloside Ⅳ inhibits lung cancer progression and metastasis by modulating macrophage polarization through AMPK signaling[J].J Exp Clin Cancer Res,2018,37:1 doi:10.1186/s13046-018-0878-0
[15] NOURI Z,FAKHRI S,NOURI K,et al.Targeting multiple signaling pathways in cancer:the rutin therapeutic approach[J].Cancers,2020,12(8):2276
[16] YANG B,YANG N,CHEN Y,et al.An integrated strategy for effective-component discovery of Astragali Radix in the treatment of lung cancer[J].Front Pharmacol,2021,11:580978.doi:10.3389/fphar.2020.580978
[17] 彭勇波,李甜甜,祝小峰,等.对香豆酸抑制肺癌细胞增殖、迁移并诱导其凋亡的机制研究[J].中南民族大学学报(自然科学版),2023,42(2):180
PENG YB,LI TT,ZHU XF,et al.The mechanisms of coumaric acid inhibiting proliferation,migration and inducing apoptosis of lung cancer cells[J].J South Cent Minzu Univ(Nat Sci Ed),2023,42(2):180
[18] 刘佳芹,周立霞,陈文现,等.毛蕊异黄酮对肺腺癌SPC-A1细胞生长及凋亡的影响[J].海南医学,2023,34(07):913
LIU JQ,ZHOU LX,CHEN WX,et al.Effect of calycosin on proliferation and apoptosis of lung adenocarcinoma cell line SPC-A1 in nude mice[J].Hainan Med J,2023,34(07):913
[19] 李龙妹,黄锦鹏,河文峰,等.龙葵提取物澳洲茄碱诱导A549细胞凋亡的机制研究[J].中药新药与临床药理,2020,31(12):1422
LI LM,HUANG JP,HE WF,et al.Molecular mechanism of apoptosis induced by solasonine extracted from Solanum nigrum in A549 cells[J].Tradit Chin Drug Res Clin Pharmacol,2020,31(12):1422
[20] 曹春艳,张家祺,张立超.澳洲茄边碱抗肿瘤作用及其机制研究进展[J].中国医院药学杂志,2022,42(20):2188
CAO CY,ZHANG JQ,ZHANG LC.Research progress on antitumor effect and mechanism of solamargine[J].Chin J Hosp Pharm,2022,42(20):2188
[21] JIANG F,XU XR,LI WM,et al.Monotropein alleviates H2O2-induced inflammation,oxidative stress and apoptosis via NF-κB/AP-1 signaling[J].Mol Med Rep,2020,22(6):4828
[22] CAI MM,LIU MY,CHEN PX,et al.Iridoids with anti-inflammatory effect from the aerial parts of Morinda officinalis How[J].Fitoterapia,2021,153:104991.doi:10.1016/j.fitote.2021.104991
[23] KALTHOFF S,PAULUSCH S,RUPP A,et al.The coffee ingredients caffeic acid and caffeic acid phenylethyl ester protect against irinotecan-induced leukopenia and oxidative stress response[J].Brit J Pharmacol,2020,177(18):4193
[24] YUE SJ,ZHANG PX,ZHU Y,et al.A ferulic acid derivative FXS-3 inhibits proliferation and metastasis of human lung cancer A549 cells via positive JNK signaling pathway and negative ERK/p38,AKT/mTOR and MEK/ERK signaling pathways[J].Molecules,2019,24(11):2165
[25] LIN Q,QU M,PATRA HK,et al.Mechanistic and therapeutic study of novel anti-tumor function of natural compound imperialine for treating non-small cell lung cancer[J].J Ethnopharmacol,2020,247:112283.doi:10.1016/j.jep.2019.112283
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