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      Chemical derivatization strategies for enhancing the HPLC analytical performance of natural active triterpenoids

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          Abstract

          Triterpenoids widely exist in nature, displaying a variety of pharmacological activities. Determining triterpenoids in different matrices, especially in biological samples holds great significance. High-performance liquid chromatography (HPLC) has become the predominant method for triterpenoids analysis due to its exceptional analytical performance. However, due to the structural similarities among botanical samples, achieving effective separation of each triterpenoid proves challenging, necessitating significant improvements in analytical methods. Additionally, triterpenoids are characterized by a lack of ultraviolet (UV) absorption groups and chromophores, along with low ionization efficiency in mass spectrometry. Consequently, routine HPLC analysis suffers from poor sensitivity. Chemical derivatization emerges as an indispensable technique in HPLC analysis to enhance its performance. Considering the structural characteristics of triterpenoids, various derivatization reagents such as acid chlorides, rhodamines, isocyanates, sulfonic esters, and amines have been employed for the derivatization analysis of triterpenoids. This review comprehensively summarized the research progress made in derivatization strategies for HPLC detection of triterpenoids. Moreover, the limitations and challenges encountered in previous studies are discussed, and future research directions are proposed to develop more effective derivatization methods.

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          Highlights

          • •

            Derivatization is a very significant step in HPLC detection of triterpenoids.

          • •

            Enhancing performance of HPLC separation and sensitivity provides unique merits.

          • •

            The derivatization sites of triterpenoids are mainly –OH and –COOH.

          • •

            Derivatization reagents are acyl chlorides, rhodamines, sulfonic esters, amines, etc.

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          A comprehensive review of the therapeutic and pharmacological effects of ginseng and ginsenosides in central nervous system

          Hee-Jin Kim, Pitna Kim, Chan Young Shin (2013)
          Ginseng is one of the most widely used herbal medicines in human. Central nervous system (CNS) diseases are most widely investigated diseases among all others in respect to the ginseng’s therapeutic effects. These include Alzheimer’s disease, Parkinson’s disease, cerebral ischemia, depression, and many other neurological disorders including neurodevelopmental disorders. Not only the various types of diseases but also the diverse array of target pathways or molecules ginseng exerts its effect on. These range, for example, from neuroprotection to the regulation of synaptic plasticity and from regulation of neuroinflammatory processes to the regulation of neurotransmitter release, too many to mention. In general, ginseng and even a single compound of ginsenoside produce its effects on multiple sites of action, which make it an ideal candidate to develop multi-target drugs. This is most important in CNS diseases where multiple of etiological and pathological targets working together to regulate the final pathophysiology of diseases. In this review, we tried to provide comprehensive information on the pharmacological and therapeutic effects of ginseng and ginsenosides on neurodegenerative and other neurological diseases. Side by side comparison of the therapeutic effects in various neurological disorders may widen our understanding of the therapeutic potential of ginseng in CNS diseases and the possibility to develop not only symptomatic drugs but also disease modifying reagents based on ginseng.
          Article 0 comments Cited 81 times – based on 0 reviews     Review now
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            Identification and characterization of phenolics and terpenoids from ethanolic extracts of Phyllanthus species by HPLC-ESI-QTOF-MS/MS

            Sunil Kumar, Awantika Singh, Brijesh Kumar (2017)
            Phyllanthus species plants are a rich source of phenolics and widely used due to their medicinal properties. A liquid chromatography–tandem mass spectrometry (LC–MS/MS) method was developed using high-pressure liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (HPLC-ESI-QTOF-MS/MS) for the identification and characterization of quercetin, kaempferol, ellagic acid and their derivatives in ethanolic extracts of Phyllanthus species. The chromatographic separation was carried out on Thermo Betasil C8 column (250 mm×4.5 mm, 5 µm) using 0.1% formic acid in water and 0.1% formic acid in methanol as the mobile phase. The identification of diagnostic fragment ions and optimization of collision energies were carried out using 21 reference standards. Totally 51 compounds were identified which include 21 compounds identified and characterized unambiguously by comparison with their authentic standards and the remaining 30 were tentatively identified and characterized in ethanolic extracts of P. emblica, P. fraternus, P. amarus and P. niruri.
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              Liquid chromatography-tandem mass spectrometry assay for simultaneous measurement of estradiol and estrone in human plasma.

              Karen Nelson, Dennis J OKane, Stefan Grebe … (2004)
              Estradiol (E2) and estrone (E1) measurements form an integral part of the assessment of female reproductive function and have expanding roles in other fields. However, many E1 and E2 immunoassays have limited functional sensitivity, suffer from cross-reactivity, and display poor intermethod agreement. To overcome these problems, we developed a sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) assay for the simultaneous measurement of E1 and E2. After dansyl chloride derivatization, samples were separated by fast gradient chromatography and injected into a tandem mass spectrometer after formation of positive ions with atmospheric pressure chemical ionization. The limits of detection and quantification, recovery, linearity, precision, and reference intervals were determined, and performance was compared with several immunoassays. Total run time per sample was 5 min. The multiple-reaction monitoring ion pairs were m/z 506/171 for 3-dansyl-estradiol and m/z 504/171 for 3-dansyl-estrone. The limits of detection for E1 and E2 were 12.9 pmol/L (3.5 ng/L) and 10.3 pmol/L (2.8 ng/L), respectively. Interassay imprecision (CV) was 4-20% (n = 20). The limits of quantification (functional sensitivities) for E1 and E2 were 44.1 pmol/L (11.9 ng/L) and 23.2 pmol/L (6.3 ng/L), respectively. The assay was linear to >2200 pmol/L ( approximately 600 ng/L) for each analyte. Recoveries were 93-108% for E1 and 100-110% for E2. No cross-reactivity was observed. Method comparison with several immunoassays revealed that the latter were inaccurate and prone to interferences at low E1 and E2 concentrations. LC-MS/MS allows rapid, simultaneous, sensitive, and accurate quantification of E1 and E2 in human serum.
              Article 0 comments Cited 40 times – based on 0 reviews     Review now
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                Author and article information

                Contributors
                Pei Luo
                Lin-Sen Qing
                Journal
                Journal ID (nlm-ta): J Pharm Anal
                Journal ID (iso-abbrev): J Pharm Anal
                Title: Journal of Pharmaceutical Analysis
                Publisher: Xi'an Jiaotong University
                ISSN (Print): 2095-1779
                ISSN (Electronic): 2214-0883
                Publication date PMC-release: 08 July 2023
                Publication date (Print): March 2024
                Publication date (Electronic): 08 July 2023
                Volume: 14
                Issue: 3
                Pages: 295-307
                Affiliations
                [a ]Chengdu Institute of Biology, Chinese Academy of Sciences, Chengdu, 610041, China
                [b ]State Key Laboratory for Quality Research in Chinese Medicines, Macau University of Science and Technology, Macao, China
                [c ]Sichuan Center for Disease Control and Prevention, Chengdu, 610041, China
                [d ]University of Chinese Academy of Sciences, Beijing, 100049, China
                Author notes
                [∗ ]Corresponding author. qingls@ 123456cib.ac.cn
                [∗∗ ]Corresponding author. pluo@ 123456must.edu.mo
                [1]

                Both authors contributed equally to this work.

                Article
                Publisher Item ID: S2095-1779(23)00141-7
                DOI: 10.1016/j.jpha.2023.07.004
                PMC ID: 11010456
                SO-VID: cbbeabce-ef0d-45dd-a6a8-9e647c706614
                Copyright © © 2023 The Authors
                License:

                This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

                History
                Date received : 10 April 2023
                Date revision received : 6 July 2023
                Date accepted : 6 July 2023
                Categories
                Subject: Review Paper

                Keywords: triterpenoid,hplc,derivatization,quantification
                Data availability:
                Keywords: triterpenoid, hplc, derivatization, quantification

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