Phytochemical Analysis最新文献

{"title":"Development and validation of a DLLME‐HPLC‐FLD method for determination of aflatoxins in Chrysanthemum morifolium based on quality by design principles","authors":"Linlin Wu, Meixu Chen, Xinyi Huo, Qilin Xu, Xianggang Yin, Xiao Han Zhao, Yifeng Zhou, Jun Huang","doi":"10.1002/pca.3445","DOIUrl":"https://doi.org/10.1002/pca.3445","url":null,"abstract":"IntroductionAflatoxins, potent carcinogens produced by Aspergillus species, present significant health risks and commonly contaminate herbal products such as <jats:styled-content style=\"fixed-case\"><jats:italic>Chrysanthemum morifolium</jats:italic></jats:styled-content>. Detecting these toxins in <jats:styled-content style=\"fixed-case\"><jats:italic>C. morifolium</jats:italic></jats:styled-content> proves challenging due to the complex nature of the herbal matrix and the fluctuating levels of toxins found in different samples.ObjectivesThis study aimed to develop and optimize a novel method for the detection of aflatoxins in <jats:styled-content style=\"fixed-case\"><jats:italic>C. morifolium</jats:italic></jats:styled-content> using dispersive liquid–liquid microextraction combined with high‐performance liquid chromatography‐fluorescence detection based on quality by design principles.MethodologyThe method involved determining critical method attributes and parameters through the Plackett–Burman design, followed by optimization using the Box–Behnken design. Monte Carlo simulation was employed to establish a design space, which was experimentally verified. Method validation was performed to confirm accuracy, precision, and stability.ResultsThe developed method exhibited excellent linearity (<jats:italic>R</jats:italic><jats:sup>2</jats:sup> &gt; 0.9991) for aflatoxins B<jats:sub>1</jats:sub>, B<jats:sub>2</jats:sub>, G<jats:sub>1</jats:sub>, and G<jats:sub>2</jats:sub> across a range of concentrations, with recovery rates between 85.52% and 102.01%. The validated method effectively quantified aflatoxins in <jats:styled-content style=\"fixed-case\"><jats:italic>C. morifolium</jats:italic></jats:styled-content> under different storage conditions, highlighting the impact of temperature and storage time on aflatoxin production.ConclusionThis study successfully established a reliable and effective method for the detection of aflatoxins in <jats:styled-content style=\"fixed-case\"><jats:italic>C. morifolium</jats:italic></jats:styled-content>, highlighting the importance of strict storage conditions to reduce aflatoxin contamination. Using a quality by design framework, the method demonstrated robustness and high analytical performance, making it suitable for routine quality control of herbal products.","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":"113 1","pages":""},"PeriodicalIF":3.3,"publicationDate":"2024-09-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142223034","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Proanthocyanidins as the marker of amomum fruit from three botanical origins based on comprehensive profiling with LC–MS and GC–MS combined with chemometrics","authors":"Kai Deng, Huali Long, Qingqing He, Jinjun Hou, Zijia Zhang, Jing Zhou, Yang Zhou, Minmin Shen, Qiang Yan, Wanying Wu","doi":"10.1002/pca.3450","DOIUrl":"https://doi.org/10.1002/pca.3450","url":null,"abstract":"IntroductionAmomum fruit, also known as Sharen, serves as both a functional food and a traditional Chinese medicine with significant pharmacological activities. However, there are three botanical origins of Amomum fruit: <jats:italic>Amomum villosum</jats:italic> Lour. (AVL), <jats:italic>Amomum villosum</jats:italic> Lour. var. <jats:italic>xanthioides</jats:italic> T. L. (AVX), and <jats:italic>Amomum longiligulare</jats:italic> T. L. Wu (ALW).ObjectiveConducting a comprehensive chemical composition analysis of Amomum fruit from three botanical origins aims to identify potential differences in metabolic characteristics.MethodsTo annotate the metabolic characteristic ions of multi‐origin Amomum fruit, we employed metabolomic techniques, including ultra‐high‐performance liquid chromatography (LC) coupled with linear ion trap‐Orbitrap–tandem mass spectrometry (MS) and gas chromatography–MS, in conjunction with feature‐based molecular networking technology. Additionally, chemometrics was utilized to examine the correlations between the various botanical origins.ResultsA total of 201 non‐volatile and 151 volatile metabolites were annotated, and most of the proanthocyanidins and flavonoids were identified by feature‐based molecular networking. Additionally, 61 non‐volatile and 45 volatile feature ions were screened out for classification. Principal component analysis, orthogonal projection to latent structures discrimination analysis, and heat map analysis were employed to clearly distinguish the metabolite profiles of Amomum fruit from different origins. Hierarchical clustering analysis indicated that proanthocyanidins C1 and C2, as well as proanthocyanins oligomers, show significant differential expression between AVX and AVL, which could be the new quality markers for the classification.ConclusionClassification of the botanical origin of Amomum fruit based on LC–MS characteristic ions proved to be more advantageous. This study introduces new strategies and technical support for the quality control of Amomum fruit and facilitates the identification of unknown compounds for future research.","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":"45 1","pages":""},"PeriodicalIF":3.3,"publicationDate":"2024-09-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142223035","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Comparative chemometric modeling of fresh and dry cannabis inflorescences using FT‐NIR spectroscopy: Quantification and classification insights","authors":"Matan Birenboim, Nimrod Brikenstein, David Kenigsbuch, Jakob A. Shimshoni","doi":"10.1002/pca.3449","DOIUrl":"https://doi.org/10.1002/pca.3449","url":null,"abstract":"Introduction<jats:styled-content style=\"fixed-case\"><jats:italic>Cannabis sativa</jats:italic></jats:styled-content> L. inflorescences are rich in cannabinoids and terpenes. Traditional chemical analysis methods for cannabinoids and terpenes, such as liquid and gas chromatography (using UV or MS detectors), are expensive and time‐consuming.ObjectivesThis study explores the use of Fourier transform near‐infrared (FT‐NIR) spectroscopy combined with chemometric approaches for classifying cannabis chemovars and predicting cannabinoid and terpene concentrations for the first time in freshly harvested (wet) cannabis inflorescence. The study also compares the performance of FT‐NIR spectroscopy on wet versus dry cannabis inflorescences.Materials and methodsSpectral data from 187 samples across seven cannabis chemovars were analyzed using partial least squares‐discriminant analysis (PLS‐DA) and partial least squares‐regression (PLS‐R) models.ResultsThe PLS‐DA models effectively classified chemovars and major classes using only two latent variables (LVs) with minimal overfitting risk, with sensitivity, specificity, and accuracy values approaching 1. Despite the high water content in wet cannabis inflorescence, the PLS‐R models demonstrated good to excellent predictive capabilities for nine cannabinoids and eight terpenes using FT‐NIR spectra for the first time, achieving cross‐validation and prediction <jats:italic>R</jats:italic>‐squared values greater than 0.7, ratio of performance to interquartile range (RPIQ) exceeding 2, and a RMSECV/RMSEC ratio below 1.24. However, the low‐cannabidiolic acid submodel and (−)‐Δ9‐trans‐tetrahydrocannabinol model showed poor predictive performance. Some cannabinoid and terpene prediction models in wet cannabis inflorescence exhibited lower predictive capabilities compared with previously published models for dry cannabis inflorescence.ConclusionsThese findings suggest that FT‐NIR spectroscopy can be a viable rapid on‐site analytical tool for growers during the inflorescence flowering stage.","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":"29 1","pages":""},"PeriodicalIF":3.3,"publicationDate":"2024-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142223067","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Comparative metabolites profiling of different solvent extracts of Asparagus species cladodes using liquid chromatography–mass spectrometry‐based metabolomics and molecular networking","authors":"Pfano W. Maphari, Mthokozisi B. C. Simelane, Ntakadzeni E. Madala, Msizi I. Mhlongo","doi":"10.1002/pca.3446","DOIUrl":"https://doi.org/10.1002/pca.3446","url":null,"abstract":"Introduction<jats:italic>Asparagus</jats:italic> species are naturally distributed worldwide and are known for their pharmacological properties that offer cures for various ailments. However, the metabolic choreography of these <jats:italic>Asparagus</jats:italic> species is not well characterized, and the compounds contributing to their bioactivities remain unknown.ObjectiveThis study aimed to profile and compare the metabolomes of three <jats:italic>Asparagus</jats:italic> species cladodes using different solvent extractions.MethodsAn ultra‐high performance liquid chromatography–quadrupole time‐of‐flight mass spectrometry‐based metabolomics and molecular networking approach was used to study the effects of different solvents (ethyl acetate, methanol, and chloroform) with varying polarity on metabolites extraction and identification of bioactive compounds from three <jats:italic>Asparagus</jats:italic> species cladodes (<jats:styled-content style=\"fixed-case\"><jats:italic>Asparagus falcatus</jats:italic></jats:styled-content>, <jats:styled-content style=\"fixed-case\"><jats:italic>Asparagus plumosus</jats:italic></jats:styled-content>, and <jats:styled-content style=\"fixed-case\"><jats:italic>Asparagus densiflorus</jats:italic></jats:styled-content> ‘Meyersii’).ResultsMultivariate statistical analyses (mainly principal component analysis) revealed a significant separation between the three solvents and the three species, indicating notable metabolic differences. A total of 118 metabolites were identified in the three species extracted with the different solvents, with methanolic and chloroform extracts containing more metabolites compared with ethyl acetate extracts. These metabolites were identified as belonging to the flavonoids, cinnamic acids, organooxygen compounds, steroids, fatty acids, benzenes, and glycerophospholipids compound classes. Furthermore, these compounds classes were differentially distributed among the three species, indicating chemical/chemotaxis differences between the compared species. Chloroform and methanol are recommended as the optimal solvents to obtain a high content of phytochemical compounds from <jats:italic>Asparagus</jats:italic> species cladodes.","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":"59 1","pages":""},"PeriodicalIF":3.3,"publicationDate":"2024-09-10","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142223036","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Feature-based molecular networking and MS2LDA analysis for the dereplication of adjacent bis-tetrahydrofuran Annonaceous acetogenins.","authors":"Aleksandra Gurgul, Chun-Tao Che","doi":"10.1002/pca.3444","DOIUrl":"https://doi.org/10.1002/pca.3444","url":null,"abstract":"<p><strong>Introduction: </strong>Annonaceous acetogenins are a group of natural polyketide compounds possessing notable cytotoxic and antitumor properties. Mass spectrometry (MS) techniques can be used for the structural determination of these compounds, including the location of functional groups along the long alkyl chain.</p><p><strong>Objective: </strong>This study aims to develop a convenient liquid chromatography (LC)-MS-based method for the dereplication of acetogenins in plant extracts using a molecular networking approach.</p><p><strong>Methodology: </strong>The LC-electrospray ionization (ESI)-MS/MS spectra of pure adjacent bis-tetrahydrofuran (THF) acetogenins isolated from Uvaria rufa (Annonaceae) were acquired, along with those of the crude ethyl acetate and hexanes fractions of the plant extract, followed by dereplication and molecular networking analysis using the Global Natural Products Social Molecular Networking (GNPS) platform.</p><p><strong>Results: </strong>A high level of fragmentation of the protonated molecules [M + H]⁺ was observed at collision energies of 37.5 and 25.0 eV. The application of feature-based molecular networking (FBMN) allowed for distinguishing diastereoisomers based on different retention times in the reversed-phase high-performance liquid chromatography method. The acetogenin possessing one or more additional OH groups on the methyl-terminal chain side of the OH-flanked bis-THF ring unit were grouped separately from those lacking such substructure. Furthermore, the MS2LDA analysis revealed shared Mass2Motifs among acetogenins, confirming the structural relations within the molecular network.</p><p><strong>Conclusions: </strong>The ESI-MS/MS-based molecular networking method provided an effective strategy for the dereplication of acetogenins in plant extracts. It is anticipated that this molecular networking approach could be extended to other types of acetogenins to facilitate rapid identification of this class of compounds.</p>","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":" ","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142133460","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"TLC-bioautography-guided identification and assessment of the antibacterial compounds from Feijoa sellowiana.","authors":"Wenliang Xu, Danxia Shi, Kuanmin Chen, David G Popovich","doi":"10.1002/pca.3448","DOIUrl":"https://doi.org/10.1002/pca.3448","url":null,"abstract":"<p><strong>Introduction: </strong>A rapid procedure was developed for the targeted isolation and assessment of antibacterial compounds from plant-based materials. The effectiveness of this method was demonstrated using Feijoa sellowiana fruit peels.</p><p><strong>Objective: </strong>The objectives of this study are as follows: develop an efficient procedure utilizing direct thin-layer chromatography (TLC)-bioautography to facilitate the targeting, identification, and purification of antibacterial compounds from plant extracts and delineate a method based on TLC-bioautography to determine the minimum effective dose (MED), alongside a colorimetric broth microdilution aided by high-performance liquid chromatography (HPLC) for evaluating the isolated active compounds.</p><p><strong>Methodology: </strong>Active compounds were targeted using TLC-bioautography against Staphylococcus aureus, and the identification was achieved through liquid chromatography-mass spectrometry (LC-MS) combined with Compound Discoverer. Purification was carried out using a customized separation method. The structure was confirmed using nuclear magnetic resonance (NMR) spectroscopy. The MED, minimum inhibitory concentration (MIC), and minimum bactericidal concentration (MBC) were determined by two enhanced antibacterial assays.</p><p><strong>Results: </strong>The main antibacterial compound identified was flavone. A TLC-bioautography-based antibacterial assay and a colorimetric broth microdilution assisted by HPLC were described as the enhanced antibacterial assay protocols. The MED, MIC, and MBC of flavone against S. aureus were found to be 4.2-5.2 μg/cm², 225-275 μg/mL, and 550-650 μg/mL, respectively. Similarly, the MED, MIC, and MBC against Escherichia coli were determined to be 5.2-6.1 μg/cm², 325-375 μg/mL, and 375-425 μg/mL, respectively.</p><p><strong>Conclusion: </strong>This study proposed an enhanced bioassay-guided separation technique for the isolation of antibacterial compounds from plants, along with two improved methods for assessing the antibacterial efficacy of insoluble or colored compounds.</p>","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":" ","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-09-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142140795","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Insight into the compositional variation of volatile and polar compounds of Radix Bupleuri from different processing technologies by GC-MS and UHPLC-Q-TOF/MS metabolomics.","authors":"Jiaxi Li, Chengye Yan, Jiahao Li, Xin Yong, Siming Han, Xiaotong Yang, Jie Du, Huijun Xu","doi":"10.1002/pca.3426","DOIUrl":"https://doi.org/10.1002/pca.3426","url":null,"abstract":"<p><strong>Introduction: </strong>Insight into comparing key active ingredients of Radix Bupleuri (RB) based on different processing technologies is a key step to reveal the material basis of drug efficacy and a challenging task for developing traditional Chinese medicine (TCM).</p><p><strong>Objective: </strong>This work aims to establish a comprehensive comparative analysis method of TCM and its processed products, which can be used to analyze the changing trend of active components of RB before and after processing.</p><p><strong>Methods: </strong>First, RB was processed with rice vinegar, rice wine, and honey. Then, ultra-high-performance liquid chromatography (UHPLC) and gas chromatography (GC) coupled with mass spectrometry (MS) technology as well as multiple statistical analyses were used to comprehensively evaluate the compositional variation of polar and volatile compounds in RB under different processing processes. Meanwhile, in UHPLC-MS, a sequential window acquisition of all theoretical fragment ion spectral and information-dependent acquisition mutual authentication (SIMA) was developed.</p><p><strong>Results: </strong>A total of 30 polar components and 33 volatile components were identified as chemical markers (mainly type II saikosaponins, terpenes, and fatty acid esters). These may be the material basis for giving unique pharmacological activities to RB and its processed products.</p><p><strong>Conclusions: </strong>These findings provided a solid foundation for the differentiated clinical application of RB, and the SIMA method held great potential for achieving accurate analysis of TCM processing ingredients.</p>","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":" ","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-09-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142133461","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Comprehensive identification of polyphenolic metabolites in aspen knotwood by combination of 2D NMR and HPLC-HRMS.","authors":"Anna V Faleva, Danil I Falev, Aleksandra A Onuchina, Nikolay V Ulyanovskii, Dmitry S Kosyakov","doi":"10.1002/pca.3443","DOIUrl":"https://doi.org/10.1002/pca.3443","url":null,"abstract":"<p><strong>Introduction: </strong>European aspen (Populus tremula L.) knotwood contains large amounts of polyphenolic metabolites, mainly flavonoids, and can be considered as a promising industrial-scale source of valuable bioactive compounds. Valorization of knotwood extractives requires detailed information on their chemical composition and a relevant analytical methodology.</p><p><strong>Objective: </strong>This study proposes combined analytical strategy for non-targeted screening and identification of polyphenolic plant metabolites and is aimed at comprehensive characterization of knotwood extractives.</p><p><strong>Materials and methods: </strong>Aspen knotwood acetone extract with determined antioxidant activity was an object of the study. Two-dimensional NMR spectroscopy with Structure Elucidator expert system was used for preliminary search of major components and specific structures. Liquid chromatography-high-resolution mass spectrometry (HPLC-HRMS) with data-dependent MS/MS spectra acquisition was used as a complementary technique providing molecular-level characterization and identification of the detected metabolites.</p><p><strong>Results: </strong>Twenty-eight phenolic metabolites were found and identified. Among them, flavonoids, aromadendrin and naringenin, as well as their glycosylated derivatives (mainly O-glucosides) and methyl ethers, dominated. Taxifolin and its 7-O-glucoside were detected as minor components. Other detected compounds are represented by p-coumaric acid and its rutinoside and small amounts of glycosylated ferulic acid. Nineteen of the detected compounds were discovered in aspen knotwood for the first time. The results were confirmed by preparative isolation of individual compounds and NMR studies.</p><p><strong>Conclusion: </strong>The proposed analytical strategy based on 2D NMR and HPLC-HRMS can be considered a powerful tool in the analysis of plant extractives and allowed for the identification and semi-quantification of a large number of polyphenols in aspen knotwood.</p>","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":" ","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-09-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142120444","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Three-dimensional spectrochromatographic determination of chlorogenic acid in Melampyrum stenophyllum Boiss. extracts by parallel factor analysis.","authors":"Zehra Ceren Ertekin, Ayşegül Köroğlu, Erdal Dinç","doi":"10.1002/pca.3439","DOIUrl":"https://doi.org/10.1002/pca.3439","url":null,"abstract":"<p><strong>Introduction: </strong>Co-elution is a common challenge in phytochemical chromatography. Full chromatographic separation often requires extensive optimization, long analysis times, and excessive solvent use. A viable alternative could be mathematical elution of analytes using three-dimensional decomposition.</p><p><strong>Objectives: </strong>This study aimed to develop a method to determine chlorogenic acid in Melampyrum stenophyllum Boiss. extracts without complete chromatographic separation, to validate the method, and to cross-validate assay results against a classical ultra-performance liquid chromatography (UPLC) method.</p><p><strong>Methodology: </strong>Ultra-performance liquid chromatography-photodiode array (UPLC-PDA) spectrochromatograms were arranged into a three-way data cube with dimensions of time, wavelength, and sample and then decomposed using parallel factor analysis to reveal chromatographic, spectral, and concentration profiles. The chromatographic and spectral profiles were used to identify chlorogenic acid in overlapping signals. The relative concentration profile was used to quantify it in the plant extract. The assay results were statistically compared with those from an in-house classical UPLC method.</p><p><strong>Results: </strong>Chlorogenic acid was co-eluted at 1.45 min and quantified as 16.11 mg per gram dry weight of Melampyrum stenophyllum extracts (SD = 0.28), despite significant interference in a 4-min runtime. The analytical validity was confirmed by recovery calculations from standard solutions and standard addition samples (RSD < 2%), and the t-test resulted in a p-value of 0.09 (α = 0.05), indicating no significant difference between the results obtained from mathematical elution and chromatographic separation.</p><p><strong>Conclusion: </strong>Chlorogenic acid was quantified from plant material accurately despite the co-elution. Validation and cross-validation results support the method's applicability.</p>","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":" ","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-09-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142110845","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Rapid mitragynine quantification and fingerprinting of products from Mitragyna speciosa Korth. leaf (Kratom) using high-performance thin-layer chromatography.","authors":"Toveelah Hayeema, Juraithip Wungsintaweekul","doi":"10.1002/pca.3442","DOIUrl":"https://doi.org/10.1002/pca.3442","url":null,"abstract":"<p><strong>Introduction: </strong>Kratom (leaves from Mitragyna speciosa Korth.; Rubiaceae) is a herbal medicine known for its analgesic properties and psychoactive effects. Kratom in Thailand is currently legal; however, it is prohibited in some countries and considered a narcotic plant.</p><p><strong>Objective: </strong>Our aim was to establish a reliable, simple, and rapid method for quantifying mitragynine in Kratom leaves and related products through a combination of high-performance thin-layer chromatography (HPTLC) and densitometry.</p><p><strong>Methodology: </strong>A densitometric HPTLC method was developed and validated in terms of specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision, and robustness. The fingerprints of kratom leaves, Mitragyna spp., and related products were constructed.</p><p><strong>Results: </strong>For HPTLC, samples were applied to silica gel 60 F₂₅₄ plates, and the mobile phase comprised n-hexane, ethyl acetate, and triethylamine (1:1:0.15, v/v/v). Densitometric detection was carried out under ultraviolet light at a wavelength of 226 nm. The validated method exhibited a range of 14.31-143.10 μg/mL, yielding a correlation coefficient of 0.9993. Spiked recovery rates were within a range of 98.3%-100.9%, and the LOD and LOQ were 3.80 and 11.53 μg/mL, respectively. Kratom samples were analyzed with the developed method, and the correlation coefficient was 0.9641, compared to the high-performance liquid chromatography-diode-array detection (HPLC-DAD) method. The HPTLC fingerprints displayed a distinctive pattern, facilitating discrimination among different plant parts and Mitragyna spp.</p><p><strong>Conclusion: </strong>The established method offers the advantages of simplicity, ease of use, and speed of analysis, serving as a practical alternative for mitragynine quantification in kratom leaf and its related products.</p>","PeriodicalId":20095,"journal":{"name":"Phytochemical Analysis","volume":" ","pages":""},"PeriodicalIF":3.0,"publicationDate":"2024-08-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"142081254","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":3,"RegionCategory":"生物学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}