首页 > 最新文献

Talanta Open最新文献

英文 中文
A comparative study of graphene-based electrodes for electrochemical detection of visceral leishmaniasis in symptomatic and asymptomatic patients 用于电化学检测有症状和无症状患者内脏利什曼病的石墨烯基电极比较研究
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-06-22 DOI: 10.1016/j.talo.2024.100339
Beatriz R. Martins , Cristhianne Molinero R. Andrade , Guilherme F. Simão , Rhéltheer de Paula Martins , Luana Barbosa Severino , Sarah Cristina Sato Vaz Tanaka , Loren Q. Pereira , Marcos Vinicius da Silva , Fernanda Bernadelli de Vito , Carlo José Freire de Oliveira , Helio Moraes de Souza , Anderson Barbosa Lima , Virmondes Rodrigues Júnior , José Roberto Siqueira Junior , Renata Pereira Alves

Background

Visceral Leishmaniasis is a neglected tropical disease with a high rate of infection and mortality in affected areas. Around 50,000 to 90,000 new cases of visceral leishmaniasis (VL) are estimated every year. Individuals asymptomatic for the disease should also be considered in epidemiological surveillance of the disease, as they can help spread the parasite. Thus, the development of low-cost diagnosis methods that allow the identification of infected and asymptomatic individuals is required, especially in developing countries where this disease is endemic.

Results

In this work, we developed an immunosensor for recognizing anti-Leishmania antibodies in asymptomatic individuals and avoiding cross-reaction with Chagas disease (CD). For that, we used carbon-based screen-printed electrodes, modified with graphene oxide and gold. Reproducibility was assessed by calculating the relative standard deviation (RSD < 5 %) from cyclic voltammograms of [Fe(CN)6]3-/4− using three different electrodes, screen-printed carbon electrodes (DPR-110) and graphene modified screen-printed electrodes (DPR-110 GPH) were purchased from DropSens (Oviedo, Asturias, Spain).

Significance

As an electrochemical methodology, we use cyclic voltammetry. After the tests were carried out, we considered that carbon electrodes adsorbed with reduced graphene oxide and modified with gold nanoparticles were the best platforms for detecting anti-Leishmania antibodies. In the study carried out, the limit of quantification (LOQ) for anti-Leishmania antibodies was established at 16.75 mg/mL, while the limit of detection (LOD) was 5.58 mg/mL. These limits indicate the minimum antibody concentration values that can be quantified and detected accurately and reliably in the analyzed sera.

背景内脏利什曼病是一种被忽视的热带疾病,在疫区的感染率和死亡率都很高。据估计,内脏利什曼病(VL)每年新增病例约 50,000 至 90,000 例。在对该疾病进行流行病学监测时,还应考虑无症状的人,因为他们可能帮助传播寄生虫。因此,特别是在这种疾病流行的发展中国家,需要开发能够识别感染者和无症状者的低成本诊断方法。结果在这项工作中,我们开发了一种免疫传感器,用于识别无症状者体内的抗利什曼病抗体,并避免与恰加斯病(CD)发生交叉反应。为此,我们使用了用氧化石墨烯和金修饰的碳基丝网印刷电极。重复性是通过计算使用三种不同电极绘制的[Fe(CN)6]3-/4-循环伏安图的相对标准偏差(RSD < 5 %)来评估的,这三种电极是丝网印刷碳电极(DPR-110)和石墨烯修饰丝网印刷电极(DPR-110 GPH),均购自 DropSens 公司(西班牙,阿斯图里亚斯,奥维耶多)。经过测试,我们认为吸附了还原氧化石墨烯并修饰了金纳米颗粒的碳电极是检测抗利什曼病抗体的最佳平台。在所进行的研究中,抗利什曼病抗体的定量限(LOQ)被确定为 16.75 mg/mL,而检测限(LOD)为 5.58 mg/mL。这些限值表明在分析的血清中可以准确可靠地定量和检测的最小抗体浓度值。
{"title":"A comparative study of graphene-based electrodes for electrochemical detection of visceral leishmaniasis in symptomatic and asymptomatic patients","authors":"Beatriz R. Martins ,&nbsp;Cristhianne Molinero R. Andrade ,&nbsp;Guilherme F. Simão ,&nbsp;Rhéltheer de Paula Martins ,&nbsp;Luana Barbosa Severino ,&nbsp;Sarah Cristina Sato Vaz Tanaka ,&nbsp;Loren Q. Pereira ,&nbsp;Marcos Vinicius da Silva ,&nbsp;Fernanda Bernadelli de Vito ,&nbsp;Carlo José Freire de Oliveira ,&nbsp;Helio Moraes de Souza ,&nbsp;Anderson Barbosa Lima ,&nbsp;Virmondes Rodrigues Júnior ,&nbsp;José Roberto Siqueira Junior ,&nbsp;Renata Pereira Alves","doi":"10.1016/j.talo.2024.100339","DOIUrl":"https://doi.org/10.1016/j.talo.2024.100339","url":null,"abstract":"<div><h3>Background</h3><p>Visceral Leishmaniasis is a neglected tropical disease with a high rate of infection and mortality in affected areas. Around 50,000 to 90,000 new cases of visceral leishmaniasis (VL) are estimated every year. Individuals asymptomatic for the disease should also be considered in epidemiological surveillance of the disease, as they can help spread the parasite. Thus, the development of low-cost diagnosis methods that allow the identification of infected and asymptomatic individuals is required, especially in developing countries where this disease is endemic.</p></div><div><h3>Results</h3><p>In this work, we developed an immunosensor for recognizing anti-<em>Leishmania</em> antibodies in asymptomatic individuals and avoiding cross-reaction with Chagas disease (CD). For that, we used carbon-based screen-printed electrodes, modified with graphene oxide and gold. Reproducibility was assessed by calculating the relative standard deviation (RSD &lt; 5 %) from cyclic voltammograms of [Fe(CN)<sub>6</sub>]<sup>3-/4−</sup> using three different electrodes, screen-printed carbon electrodes (DPR-110) and graphene modified screen-printed electrodes (DPR-110 GPH) were purchased from DropSens (Oviedo, Asturias, Spain).</p></div><div><h3>Significance</h3><p>As an electrochemical methodology, we use cyclic voltammetry. After the tests were carried out, we considered that carbon electrodes adsorbed with reduced graphene oxide and modified with gold nanoparticles were the best platforms for detecting anti-<em>Leishmania</em> antibodies. In the study carried out, the limit of quantification (LOQ) for anti-<em>Leishmania</em> antibodies was established at 16.75 mg/mL, while the limit of detection (LOD) was 5.58 mg/mL. These limits indicate the minimum antibody concentration values that can be quantified and detected accurately and reliably in the analyzed sera.</p></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":null,"pages":null},"PeriodicalIF":4.1,"publicationDate":"2024-06-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666831924000535/pdfft?md5=3a5c025abc51eb793d21087d7697fa40&pid=1-s2.0-S2666831924000535-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141481110","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Sensitive and selective colorimetric sensor detection of Sn (II): An aqueous, paper, and gel-based method by green biomimetic silver nanoparticles 灵敏和选择性比色传感器检测锡 (II):基于绿色仿生银纳米颗粒的水基、纸基和凝胶基方法
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-06-21 DOI: 10.1016/j.talo.2024.100340
Mariha Zulfa Risana , Sigit Priatmoko , Indri Yati , Zetryana Puteri Tachrim , Agustina Sus Andreani

Tin contamination in waters due to mining and natural activities in high concentrations can threaten human health. This research presents the development of a sensitive and selective colorimetric sensor in aqueous, paper, and gel-based to detect Sn2+. The development of such sensors is promising, with attractive advantages such as intense color, fast naked-eye response, and simple continuous fabrication. The addition of Sn2+ ions will change the color of the medium because curcumin (Cur) interacts with Sn2+, causing a decrease in free Cur, silver nanoparticles (AgNPs) becoming less stable, and a change in particle size. Colorimetric changes in Sn2+ were achieved by visual inspection within 10 min for aqueous-based and 20 min for paper and gel-based. The good linear relationship (R2 = 0.9999) between Sn2+ and Δ absorption with a detection limit of up to 66.99 µg/L. This method is relatively scalable in determining Sn2+ and shows good recovery between 80 and 105 %. This colorimetric sensor gives good sensitivity to Sn2+ metal ions which is expected to become the basic technology for developing in-situ sensors to monitor Sn2+ levels in tin industrial waste.

由于采矿和自然活动造成的高浓度锡污染会威胁人类健康。本研究介绍了一种灵敏且具有选择性的水基、纸基和凝胶基比色传感器,用于检测 Sn2+。这类传感器具有色彩鲜艳、肉眼反应迅速、连续制造简单等诱人优势,开发前景广阔。Sn2+ 离子的加入会改变介质的颜色,因为姜黄素(Cur)会与 Sn2+ 发生作用,导致游离的姜黄素减少、银纳米粒子(AgNPs)变得不稳定以及粒度发生变化。通过目测,水基和纸基分别在 10 分钟和 20 分钟内实现了 Sn2+ 的色度变化。Sn2+ 与 Δ 吸收之间具有良好的线性关系(R2 = 0.9999),检测限高达 66.99 µg/L。该方法在测定 Sn2+ 方面具有较强的可扩展性,回收率在 80% 到 105% 之间。这种比色传感器对 Sn2+ 金属离子具有良好的灵敏度,有望成为开发原位传感器监测锡工业废物中 Sn2+ 含量的基本技术。
{"title":"Sensitive and selective colorimetric sensor detection of Sn (II): An aqueous, paper, and gel-based method by green biomimetic silver nanoparticles","authors":"Mariha Zulfa Risana ,&nbsp;Sigit Priatmoko ,&nbsp;Indri Yati ,&nbsp;Zetryana Puteri Tachrim ,&nbsp;Agustina Sus Andreani","doi":"10.1016/j.talo.2024.100340","DOIUrl":"https://doi.org/10.1016/j.talo.2024.100340","url":null,"abstract":"<div><p>Tin contamination in waters due to mining and natural activities in high concentrations can threaten human health. This research presents the development of a sensitive and selective colorimetric sensor in aqueous, paper, and gel-based to detect Sn<sup>2+</sup>. The development of such sensors is promising, with attractive advantages such as intense color, fast naked-eye response, and simple continuous fabrication. The addition of Sn<sup>2+</sup> ions will change the color of the medium because curcumin (Cur) interacts with Sn<sup>2+</sup>, causing a decrease in free Cur, silver nanoparticles (AgNPs) becoming less stable, and a change in particle size. Colorimetric changes in Sn<sup>2+</sup> were achieved by visual inspection within 10 min for aqueous-based and 20 min for paper and gel-based. The good linear relationship (R<sup>2</sup> = 0.9999) between Sn<sup>2+</sup> and Δ absorption with a detection limit of up to 66.99 µg/L. This method is relatively scalable in determining Sn<sup>2+</sup> and shows good recovery between 80 and 105 %. This colorimetric sensor gives good sensitivity to Sn<sup>2+</sup> metal ions which is expected to become the basic technology for developing in-situ sensors to monitor Sn<sup>2+</sup> levels in tin industrial waste.</p></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":null,"pages":null},"PeriodicalIF":4.1,"publicationDate":"2024-06-21","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666831924000547/pdfft?md5=32f84a451f8fc81bad4a56e566bf77b3&pid=1-s2.0-S2666831924000547-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141481111","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Analysis of major cannabinoids using Raman microscopy, density functional theory, chemometrics and a novel artificial intelligence approach 利用拉曼显微镜、密度泛函理论、化学计量学和新型人工智能方法分析主要大麻素
IF 4.1 Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-06-20 DOI: 10.1016/j.talo.2024.100337
Jose Grijalva , Ting-Yu Huang , Jorn Yu , Patrick Buzzini , Darren Williams , J. Tyler Davidson , Geraldine Monjardez

With a rise in the prominence of cannabis usage, due to its widespread availability and varying legal status, there has been an increased emphasis on the differentiation of cannabinoids present within cannabis using various analytical techniques. The present study aimed to exploit the capability of Raman microscopy to collect high-quality spectra of seven cannabinoid analytical standards, followed by their classification using linear discriminant analysis (LDA) and a novel transfer learning approach. Additionally, the experimental Raman spectra of delta-9-tetrahydrocannabinol (Δ9-THC), cannabidiol (CBD), and cannabichromene (CBC) were compared to simulated spectra from density functional theory calculations (DFT) to connect the spectral features to the underlying vibrational motions. A microscopical approach enabled the determination of the optimal sampling areas to collect Raman spectra for the nonacidic and acidic cannabinoids. An initial visualization of the data using principal component analysis (PCA) confirmed the spectral differences observable by visual comparisons of the spectra of the cannabinoid standards. The application of LDA implemented with a 5-fold cross-validation with 10 repeats, resulted in a classification accuracy of 99.83 %. For the transfer learning approach, the artificial intelligence (AI) model training was conducted in less than 10 min in a graphical processing unit (GPU) environment. All seven cannabinoids were successfully classified into respective classes based on scalograms transformed from Raman spectra, with 100 % classification accuracy. The average prediction probability for correct classification was 99.31 %. The classification outcome provided by the AI model included both prediction labels and probability, which provided a comprehensive evaluation of the samples.

由于大麻的广泛供应和不同的法律地位,大麻的使用日益突出,因此人们越来越重视利用各种分析技术对大麻中的大麻素进行区分。本研究旨在利用拉曼显微镜的能力收集七种大麻素分析标准的高质量光谱,然后利用线性判别分析(LDA)和新型迁移学习方法对其进行分类。此外,还将δ-9-四氢大麻酚(Δ9-THC)、大麻二酚(CBD)和大麻色烯(CBC)的实验拉曼光谱与密度泛函理论计算(DFT)的模拟光谱进行了比较,以便将光谱特征与基本振动运动联系起来。采用显微镜方法确定了收集非酸性和酸性大麻素拉曼光谱的最佳取样区域。使用主成分分析(PCA)对数据进行初步可视化,证实了通过目测比较大麻素标准物质的光谱可以观察到的光谱差异。应用 LDA 进行 10 次重复的 5 倍交叉验证后,分类准确率达到 99.83%。在迁移学习方法中,人工智能(AI)模型的训练是在图形处理器(GPU)环境下进行的,用时不到 10 分钟。根据从拉曼光谱转换而来的扫描图,所有七种大麻素都成功地被归入了各自的类别,分类准确率达到 100%。正确分类的平均预测概率为 99.31%。人工智能模型提供的分类结果包括预测标签和概率,对样本进行了全面评估。
{"title":"Analysis of major cannabinoids using Raman microscopy, density functional theory, chemometrics and a novel artificial intelligence approach","authors":"Jose Grijalva ,&nbsp;Ting-Yu Huang ,&nbsp;Jorn Yu ,&nbsp;Patrick Buzzini ,&nbsp;Darren Williams ,&nbsp;J. Tyler Davidson ,&nbsp;Geraldine Monjardez","doi":"10.1016/j.talo.2024.100337","DOIUrl":"https://doi.org/10.1016/j.talo.2024.100337","url":null,"abstract":"<div><p>With a rise in the prominence of cannabis usage, due to its widespread availability and varying legal status, there has been an increased emphasis on the differentiation of cannabinoids present within cannabis using various analytical techniques. The present study aimed to exploit the capability of Raman microscopy to collect high-quality spectra of seven cannabinoid analytical standards, followed by their classification using linear discriminant analysis (LDA) and a novel transfer learning approach. Additionally, the experimental Raman spectra of delta-9-tetrahydrocannabinol (Δ9-THC), cannabidiol (CBD), and cannabichromene (CBC) were compared to simulated spectra from density functional theory calculations (DFT) to connect the spectral features to the underlying vibrational motions. A microscopical approach enabled the determination of the optimal sampling areas to collect Raman spectra for the nonacidic and acidic cannabinoids. An initial visualization of the data using principal component analysis (PCA) confirmed the spectral differences observable by visual comparisons of the spectra of the cannabinoid standards. The application of LDA implemented with a 5-fold cross-validation with 10 repeats, resulted in a classification accuracy of 99.83 %. For the transfer learning approach, the artificial intelligence (AI) model training was conducted in less than 10 min in a graphical processing unit (GPU) environment. All seven cannabinoids were successfully classified into respective classes based on scalograms transformed from Raman spectra, with 100 % classification accuracy. The average prediction probability for correct classification was 99.31 %. The classification outcome provided by the AI model included both prediction labels and probability, which provided a comprehensive evaluation of the samples.</p></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":null,"pages":null},"PeriodicalIF":4.1,"publicationDate":"2024-06-20","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666831924000511/pdfft?md5=1cb9dd2a4e5bf89067296982964c0626&pid=1-s2.0-S2666831924000511-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141444392","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Paper based analytical platforms: A matrix adaptable approach to drug testing 基于纸张的分析平台:药物检测的矩阵适应性方法
IF 4.1 Q3 Chemistry Pub Date : 2024-06-18 DOI: 10.1016/j.talo.2024.100338
Naga Prashant Koppuravuri, Suvarna Yenduri, Rukaiya Nabi, Pooja M, Aishwarya N, Sanika M, Sinchana Prakash

Paper-based analytical devices (PADs) are becoming increasingly popular for drug analysis in various matrices. These affordable, portable platforms come with a range of benefits, such as their user-friendly design, straightforward operation, and minimal need for sample preparation. This study evaluates the potential applications of PADs in drug testing with a particular emphasis on the adaptability of PADs in terms of their ability to handle various types of samples during the testing process. In this study, the design, manufacturing, and performance of PADs for drug detection, as well as the influence that different biological samples have on the performance of PAD performance were investigated. PADs are discussed in this paper, with respect to their applications in forensic sample analysis, point-of-care testing and illicit drug testing. The study demonstrates the flexibility of PADs as platforms for drug testing in varied matrices. The authors highlight the fact that PADs are inexpensive, portable, user-friendly, and need minimum sample preparation, which makes them effective instruments in a variety of situations, including research, law enforcement, and healthcare. On the whole, this paper highlights the versatility of PADs, emphasizing their role as adaptable platforms for drug testing within different matrices. Scientists and professionals can utilize these cutting-edge devices to improve the efficiency and accessibility of drug analysis.

纸质分析装置(PAD)在各种基质的药物分析中越来越受欢迎。这些经济实惠的便携式平台具有一系列优点,如设计方便用户、操作简单、样品制备的需求极低。本研究评估了 PAD 在药物检测中的潜在应用,特别强调了 PAD 在检测过程中处理各类样品的适应性。本研究调查了用于药物检测的 PAD 的设计、制造和性能,以及不同生物样本对 PAD 性能的影响。本文讨论了 PAD 在法医样本分析、护理点检测和非法药物检测中的应用。研究证明了 PAD 作为不同基质中药物检测平台的灵活性。作者强调,PAD 价格低廉、便于携带、使用方便,只需最少的样品制备,因此是研究、执法和医疗保健等各种情况下的有效仪器。总体而言,本文突出了 PAD 的多功能性,强调了其作为在不同基质中进行药物检测的适应性平台的作用。科学家和专业人员可以利用这些尖端设备来提高药物分析的效率和便利性。
{"title":"Paper based analytical platforms: A matrix adaptable approach to drug testing","authors":"Naga Prashant Koppuravuri,&nbsp;Suvarna Yenduri,&nbsp;Rukaiya Nabi,&nbsp;Pooja M,&nbsp;Aishwarya N,&nbsp;Sanika M,&nbsp;Sinchana Prakash","doi":"10.1016/j.talo.2024.100338","DOIUrl":"https://doi.org/10.1016/j.talo.2024.100338","url":null,"abstract":"<div><p>Paper-based analytical devices (PADs) are becoming increasingly popular for drug analysis in various matrices. These affordable, portable platforms come with a range of benefits, such as their user-friendly design, straightforward operation, and minimal need for sample preparation. This study evaluates the potential applications of PADs in drug testing with a particular emphasis on the adaptability of PADs in terms of their ability to handle various types of samples during the testing process. In this study, the design, manufacturing, and performance of PADs for drug detection, as well as the influence that different biological samples have on the performance of PAD performance were investigated. PADs are discussed in this paper, with respect to their applications in forensic sample analysis, point-of-care testing and illicit drug testing. The study demonstrates the flexibility of PADs as platforms for drug testing in varied matrices. The authors highlight the fact that PADs are inexpensive, portable, user-friendly, and need minimum sample preparation, which makes them effective instruments in a variety of situations, including research, law enforcement, and healthcare. On the whole, this paper highlights the versatility of PADs, emphasizing their role as adaptable platforms for drug testing within different matrices. Scientists and professionals can utilize these cutting-edge devices to improve the efficiency and accessibility of drug analysis.</p></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":null,"pages":null},"PeriodicalIF":4.1,"publicationDate":"2024-06-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666831924000523/pdfft?md5=17165c68016095cd1810eac3322939f9&pid=1-s2.0-S2666831924000523-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141444391","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Development of a liquid chromatographic method with a different selectivity for the quantification of eighteen phytocannabinoids in hemp 开发一种具有不同选择性的液相色谱法,用于定量分析大麻中的十八种植物大麻素
Q3 Chemistry Pub Date : 2024-06-06 DOI: 10.1016/j.talo.2024.100336
Liguo Song, Jake Provis, Ammar Mohammad Al-Bataineh, Keszia Jervelle Fabien, Madeline Kotler

To quantify phytocannabinoids in hemp, liquid chromatography diode array detector (LC-DAD) methods are favored, but their selectivity depends on baseline separation of all phytocannabinoids and unknown compounds in an extract. Therefore, development of a LC-DAD method with a different selectivity has become highly desirable. Currently, most LC-DAD methods use the water/acetonitrile eluting system, while this study aimed to use the water/methanol eluting system. A systematic investigation of various chromatographic parameters on LC separation of eighteen phytocannabinoids, the maximum number that has been quantified in hemp so far, plus two potential internal standards, led to a four-step isocratic mobile phase that was able to baseline separate the twenty compounds with a significantly different eluting order from published methods. Although changes in the mobile phase composition caused baseline drifts, consequent difficulty in quantification was avoided through detection at wavelengths longer than 230 nm. Subsequently, the method was validated according to the ISO 17025 guidelines, calibrated between 0.04 and 50 µg/mL, and used to analyze phytocannabinoids in nine strains of hemp flowers that were extracted using methanol between 0.04 and 50 % (w/w). Extraction recovery was tracked in real-time by spiking one of the two potential internal standards, i.e., abnormal cannabidiol (ACBD), a cannabinoid not naturally present in hemp. Method selectivity was further assessed by electrospray ionization time-of-flight mass spectrometry (ESI/TOFMS), indicating minimum interferences. In addition, five untargeted/unknown phytocannabinoids were identified by ESI/TOFMS, including two structural isomers of Δ9-tetrahydrocannabinol (Δ9-THC), two structural isomers of Δ9-tetrahydrocannabinolic acid (Δ9-THCA), and one structural isomer of Δ9-THC acetate.

为了量化大麻中的植物大麻素,液相色谱二极管阵列检测器(LC-DAD)方法受到青睐,但其选择性取决于提取物中所有植物大麻素和未知化合物的基线分离。因此,开发一种具有不同选择性的 LC-DAD 方法已成为当务之急。目前,大多数 LC-DAD 方法使用水/乙腈洗脱系统,而本研究旨在使用水/甲醇洗脱系统。通过对 18 种植物大麻素(迄今为止已在大麻中定量的最多植物大麻素)以及两种潜在内标物的 LC 分离过程中的各种色谱参数进行系统研究,最终确定了一种四步等度流动相,该流动相能够基线分离这 20 种化合物,其洗脱顺序与已发表的方法有显著不同。虽然流动相成分的变化会导致基线漂移,但通过波长长于 230 nm 的检测波长,可以避免由此造成的定量困难。随后,根据 ISO 17025 准则对该方法进行了验证,在 0.04 至 50 µg/mL 之间进行了校准,并用于分析 9 株大麻花中的植物大麻素,这些大麻花是用 0.04 至 50 %(w/w)的甲醇提取的。通过添加两种潜在内标之一(即异常大麻二酚 (ACBD),一种大麻中不天然存在的大麻素)来实时跟踪萃取回收率。电喷雾电离飞行时间质谱法(ESI/TOFMS)进一步评估了该方法的选择性,结果表明干扰最小。此外,ESI/TOFMS 还鉴定出五种未锁定/未知的植物大麻素,包括 Δ9-四氢大麻酚(Δ9-THC)的两种结构异构体、Δ9-四氢大麻酚酸(Δ9-THCA)的两种结构异构体和 Δ9-THC乙酸酯的一种结构异构体。
{"title":"Development of a liquid chromatographic method with a different selectivity for the quantification of eighteen phytocannabinoids in hemp","authors":"Liguo Song,&nbsp;Jake Provis,&nbsp;Ammar Mohammad Al-Bataineh,&nbsp;Keszia Jervelle Fabien,&nbsp;Madeline Kotler","doi":"10.1016/j.talo.2024.100336","DOIUrl":"10.1016/j.talo.2024.100336","url":null,"abstract":"<div><p>To quantify phytocannabinoids in hemp, liquid chromatography diode array detector (LC-DAD) methods are favored, but their selectivity depends on baseline separation of all phytocannabinoids and unknown compounds in an extract. Therefore, development of a LC-DAD method with a different selectivity has become highly desirable. Currently, most LC-DAD methods use the water/acetonitrile eluting system, while this study aimed to use the water/methanol eluting system. A systematic investigation of various chromatographic parameters on LC separation of eighteen phytocannabinoids, the maximum number that has been quantified in hemp so far, plus two potential internal standards, led to a four-step isocratic mobile phase that was able to baseline separate the twenty compounds with a significantly different eluting order from published methods. Although changes in the mobile phase composition caused baseline drifts, consequent difficulty in quantification was avoided through detection at wavelengths longer than 230 nm. Subsequently, the method was validated according to the ISO 17025 guidelines, calibrated between 0.04 and 50 µg/mL, and used to analyze phytocannabinoids in nine strains of hemp flowers that were extracted using methanol between 0.04 and 50 % (w/w). Extraction recovery was tracked in real-time by spiking one of the two potential internal standards, i.e., abnormal cannabidiol (ACBD), a cannabinoid not naturally present in hemp. Method selectivity was further assessed by electrospray ionization time-of-flight mass spectrometry (ESI/TOFMS), indicating minimum interferences. In addition, five untargeted/unknown phytocannabinoids were identified by ESI/TOFMS, including two structural isomers of Δ<sup>9</sup>-tetrahydrocannabinol (Δ<sup>9</sup>-THC), two structural isomers of Δ<sup>9</sup>-tetrahydrocannabinolic acid (Δ<sup>9</sup>-THCA), and one structural isomer of Δ<sup>9</sup>-THC acetate.</p></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S266683192400050X/pdfft?md5=6e331f8cd0096084d1d30fc9cc36c61d&pid=1-s2.0-S266683192400050X-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141405886","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Tandem mass spectrometry imaging to assess illudin S distributions in Omphalotus illudens mushrooms 利用串联质谱成像技术评估伊柳丁 S 在牛肝菌蘑菇中的分布情况
Q1 CHEMISTRY, ANALYTICAL Pub Date : 2024-06-03 DOI: 10.1016/j.talo.2024.100335
Shigeki Matsui , Takahiro Takayama , Koichi Inoue

Poisoning metabolites within mushrooms typically exert varying physiological and biological effects; however, their distributions within mushrooms are seldom investigated. This study focused on imaging illudin S, a representative poisoning metabolite within Omphalotus illudens mushroom, using desorption electrospray ionization–tandem mass spectrometry (DESI–MS/MS) coupled with liquid chromatography–electrospray ionization–tandem mass spectrometry (LC–ESI–MS/MS). Initially, LC–ESI–MS/MS conditions were established for the selective detection of illudin S (m/z 247→159, positive mode) from extracted mushroom. Based on this MS/MS condition, each mushroom was divided into nine sections, and each section was subjected to specific DESI–MS/MS mode imaging (pixel size: 200 × 200 μm). The results revealed high concentrations of illudin S in the stalks of the mushrooms growing on trees. Further, re-evaluations using the LC–MS/MS assay revealed a seven-fold difference in the illudin S between the stalk and other regions. This study marks the first attempt at assessing toxic metabolite distributions within poisonous mushrooms, thus offering valuable insights including the efficient utilization of illudin analogs in biological applications.

蘑菇中的中毒代谢物通常会产生不同的生理和生物效应;然而,很少有人研究它们在蘑菇中的分布情况。本研究采用解吸电喷雾离子化-串联质谱法(DESI-MS/MS)和液相色谱-电喷雾离子化-串联质谱法(LC-ESI-MS/MS),重点研究了蘑菇中具有代表性的中毒代谢物--illudin S。初步建立了从蘑菇提取物中选择性检测伊柳丁 S(m/z 247→159,阳性模式)的 LC-ESI-MS/MS 条件。在此 MS/MS 条件下,每个蘑菇被分成九个切片,每个切片进行特定的 DESI-MS/MS 模式成像(像素尺寸:200 × 200 μm)。结果显示,生长在树上的蘑菇茎秆中含有高浓度的伊柳丁 S。此外,使用 LC-MS/MS 分析法进行的重新评估显示,蘑菇柄和其他区域的菇黄素 S 含量相差七倍。这项研究首次尝试评估毒蘑菇中有毒代谢物的分布情况,从而提供了宝贵的见解,包括在生物应用中有效利用 illudin 类似物。
{"title":"Tandem mass spectrometry imaging to assess illudin S distributions in Omphalotus illudens mushrooms","authors":"Shigeki Matsui ,&nbsp;Takahiro Takayama ,&nbsp;Koichi Inoue","doi":"10.1016/j.talo.2024.100335","DOIUrl":"10.1016/j.talo.2024.100335","url":null,"abstract":"<div><p>Poisoning metabolites within mushrooms typically exert varying physiological and biological effects; however, their distributions within mushrooms are seldom investigated. This study focused on imaging illudin S, a representative poisoning metabolite within <em>Omphalotus illudens</em> mushroom, using desorption electrospray ionization–tandem mass spectrometry (DESI–MS/MS) coupled with liquid chromatography–electrospray ionization–tandem mass spectrometry (LC–ESI–MS/MS). Initially, LC–ESI–MS/MS conditions were established for the selective detection of illudin S (<em>m/z</em> 247→159, positive mode) from extracted mushroom. Based on this MS/MS condition, each mushroom was divided into nine sections, and each section was subjected to specific DESI–MS/MS mode imaging (pixel size: 200 × 200 μm). The results revealed high concentrations of illudin S in the stalks of the mushrooms growing on trees. Further, re-evaluations using the LC–MS/MS assay revealed a seven-fold difference in the illudin S between the stalk and other regions. This study marks the first attempt at assessing toxic metabolite distributions within poisonous mushrooms, thus offering valuable insights including the efficient utilization of illudin analogs in biological applications.</p></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-06-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666831924000493/pdfft?md5=6bf5c910a5b7602fb11eced0f8861fe6&pid=1-s2.0-S2666831924000493-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141275315","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Non-destructive fluorescence spectroscopy for quality evaluation of almond oils extracted from roasted kernel 用非破坏性荧光光谱法评估从烘烤果仁中提取的杏仁油的质量
Q3 Chemistry Pub Date : 2024-05-28 DOI: 10.1016/j.talo.2024.100334
Elísabet Martín-Tornero , David Simón-García , Manuel Álvarez-Ortí , José Emilio Pardo , Isabel Durán-Merás , Daniel Martín-Vertedor

Almond oils extracted from roasted kernels at different roasting times at 150 °C were analyzed to quantify quality parameters such as acidity, peroxide value, K232, K270, antioxidant activity and the oxidative stability index. The roasting process induced oxidation of the chemical compounds in the oil, resulting in increased acidity, peroxide value, K232 and K270. The antioxidant activity exhibited a decreasing trend over time, while the oxidative stability showed only slight changes. Excitation-emission matrices (EEMs) were directly scanned on almond oil samples. The combination of the EEMs with parallel factor analysis (PARAFAC) provided qualitative information about the main fluorophores and their evolution with the roasting time. Quantitative information was obtained using unfolded partial least squares (U-PLS), demonstrating the effectiveness of the fluorescence technique in combination with multivariate analysis to quantify analytical parameters in almond oils. Prediction models were developed, and subjected to external validation. The coefficients of determination in the external validation were higher than 0.94 for all parameters except k270.

分析了从 150 °C 不同烘焙时间的杏仁中提取的杏仁油,以量化酸度、过氧化值、K、K 值、抗氧化活性和氧化稳定性指数等质量参数。焙烧过程会引起油中化合物的氧化,导致酸度、过氧化值、K 值和 K 值增加。在杏仁油样品上直接扫描了激发-发射矩阵(EEM)。将激发发射矩阵与并行因子分析(PARAFAC)相结合,可获得有关主要荧光团及其随焙烧时间变化的定性信息。利用展开偏最小二乘法(U-PLS)获得了定量信息,证明了荧光技术与多元分析相结合在量化杏仁油分析参数方面的有效性。建立了预测模型,并进行了外部验证。在外部验证中,除 k270 外,所有参数的确定系数均高于 0.94。
{"title":"Non-destructive fluorescence spectroscopy for quality evaluation of almond oils extracted from roasted kernel","authors":"Elísabet Martín-Tornero ,&nbsp;David Simón-García ,&nbsp;Manuel Álvarez-Ortí ,&nbsp;José Emilio Pardo ,&nbsp;Isabel Durán-Merás ,&nbsp;Daniel Martín-Vertedor","doi":"10.1016/j.talo.2024.100334","DOIUrl":"10.1016/j.talo.2024.100334","url":null,"abstract":"<div><p>Almond oils extracted from roasted kernels at different roasting times at 150 °C were analyzed to quantify quality parameters such as acidity, peroxide value, K<sub>232</sub>, K<sub>270</sub>, antioxidant activity and the oxidative stability index. The roasting process induced oxidation of the chemical compounds in the oil, resulting in increased acidity, peroxide value, K<sub>232</sub> and K<sub>270</sub>. The antioxidant activity exhibited a decreasing trend over time, while the oxidative stability showed only slight changes. Excitation-emission matrices (EEMs) were directly scanned on almond oil samples. The combination of the EEMs with parallel factor analysis (PARAFAC) provided qualitative information about the main fluorophores and their evolution with the roasting time. Quantitative information was obtained using unfolded partial least squares (U-PLS), demonstrating the effectiveness of the fluorescence technique in combination with multivariate analysis to quantify analytical parameters in almond oils. Prediction models were developed, and subjected to external validation. The coefficients of determination in the external validation were higher than 0.94 for all parameters except k270.</p></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-28","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666831924000481/pdfft?md5=f5efd4c101389d9f573785fc65454f13&pid=1-s2.0-S2666831924000481-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141194571","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Analytical applications of europium metal-organic frameworks: A brief Overview 铕金属有机框架的分析应用:简要概述
Q3 Chemistry Pub Date : 2024-05-23 DOI: 10.1016/j.talo.2024.100329
Shubhranshu Mishra, Shiva, Surajit Rakshit, Nidhi Goel

Eu-MOFs have sparked widespread interest as a dependable, convenient, time-saving, highly sensitive, and specialised platform for analytical applications due to their strong skeletons, extremely high surface area, changeable pore sizes, easy functionalization, and great stability. This review will provide remarkable insight into the synthesis, structure, and properties of Eu-MOFs. Here, we will also focus on Eu-MOF applications as chemosensors, biosensors, selective gas adsorption, and chromatographic stationary phases in order to meet the needs of the materials used for analysis. Hence, this study will offer a comprehensive overview of existing research on the analytical applications of Eu-MOFs. We expect that this study will provide complete knowledge for researchers to recreate the procedures and contribute to future discoveries in this prominent field.

Eu-MOFs 具有骨架坚固、比表面积极高、孔径可变、易于功能化和稳定性强等特点,是一种可靠、方便、省时、高灵敏度和专业化的分析应用平台,因而引发了广泛的兴趣。本综述将对 Eu-MOFs 的合成、结构和特性提供深入的见解。在此,我们还将重点介绍 Eu-MOF 作为化学传感器、生物传感器、选择性气体吸附和色谱固定相的应用,以满足分析所用材料的需求。因此,本研究将对有关 Eu-MOFs 分析应用的现有研究进行全面概述。我们希望这项研究能为研究人员提供完整的知识,以便他们重新创建程序,并为这一重要领域的未来发现做出贡献。
{"title":"Analytical applications of europium metal-organic frameworks: A brief Overview","authors":"Shubhranshu Mishra,&nbsp;Shiva,&nbsp;Surajit Rakshit,&nbsp;Nidhi Goel","doi":"10.1016/j.talo.2024.100329","DOIUrl":"10.1016/j.talo.2024.100329","url":null,"abstract":"<div><p>Eu-MOFs have sparked widespread interest as a dependable, convenient, time-saving, highly sensitive, and specialised platform for analytical applications due to their strong skeletons, extremely high surface area, changeable pore sizes, easy functionalization, and great stability. This review will provide remarkable insight into the synthesis, structure, and properties of Eu-MOFs. Here, we will also focus on Eu-MOF applications as chemosensors, biosensors, selective gas adsorption, and chromatographic stationary phases in order to meet the needs of the materials used for analysis. Hence, this study will offer a comprehensive overview of existing research on the analytical applications of Eu-MOFs. We expect that this study will provide complete knowledge for researchers to recreate the procedures and contribute to future discoveries in this prominent field.</p></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666831924000432/pdfft?md5=72b0eafe7f4c3b59c8973dacba3014bc&pid=1-s2.0-S2666831924000432-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141135856","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Rapid screening of designer fuel frauds by Raman spectroscopy 利用拉曼光谱学快速筛查人造燃料欺诈行为
Q3 Chemistry Pub Date : 2024-05-23 DOI: 10.1016/j.talo.2024.100333
Gennaro Picardi , Fabrizio Cattaruzza , Daniela Mangione , Francesco Manzo , Alessandro Terracciano , Alessandro Proposito

Designer fuel fraud consists in the smuggling of modified diesel blends as engine lubricant oils and their illegal trade avoiding payment of the excise duty applied to energy products. The fraudulent mixture contains regular diesel fuel plus a heavier hydrocarbon fraction, originating from waste automotive lubricant or cheap, residual base oils.

Raman spectroscopy was tested as a rapid in-situ screening method to separate regular diesel fuel samples from those suspected to contain a heavier component, and thus demanding a more extensive characterization. The Raman fingerprint region from the screened sample is matched to purposely created spectral libraries of compliant and non-compliant diesel fuels using the instrumental search algorithm. Overall, 177 compliant fuel samples and 28 non-compliant samples (all designer fuels with a confirmed heavier fraction and/or anomalous distillation parameters) were measured. The designer fuels were all positively identified, with ∼18 % false positives.

Subsequently, the Raman data-set was studied by Principal Component Analysis (PCA) and then classified as either compliant or non-compliant using Linear Discriminant Analysis (LDA). PCA using up to three principal components for data visualization shows only an incipient separation but still a partial overlap between compliant and non-compliant samples. LDA, on the opposite, performed superiorly in the binary classification task, with no false negatives and less than 4 % false positives.

设计者燃料欺诈是指将改良柴油混合物作为发动机润滑油走私并进行非法贸易,以规避对能源产品征收的消费税。这种欺诈性混合物含有普通柴油和较重的碳氢化合物,这些碳氢化合物来自废弃的汽车润滑油或廉价的残留基础油。拉曼光谱是一种快速原位筛选方法,用于将普通柴油样品与疑似含有较重成分的柴油样品区分开来,因此需要进行更广泛的特征描述。利用仪器搜索算法,将筛选样品的拉曼指纹区域与特意创建的符合标准和不符合标准柴油的光谱库进行匹配。总体而言,共测量了 177 个符合标准的燃料样品和 28 个不符合标准的样品(均为已确认重馏分和/或馏分参数异常的特制燃料)。随后,通过主成分分析(PCA)对拉曼数据集进行了研究,然后使用线性判别分析(LDA)将其分为符合标准和不符合标准两种。使用多达三个主成分进行数据可视化的 PCA 显示,符合标准和不符合标准的样品之间只有初步的分离,但仍有部分重叠。相反,线性判别分析在二元分类任务中表现优异,没有误判,误判率低于 4%。
{"title":"Rapid screening of designer fuel frauds by Raman spectroscopy","authors":"Gennaro Picardi ,&nbsp;Fabrizio Cattaruzza ,&nbsp;Daniela Mangione ,&nbsp;Francesco Manzo ,&nbsp;Alessandro Terracciano ,&nbsp;Alessandro Proposito","doi":"10.1016/j.talo.2024.100333","DOIUrl":"10.1016/j.talo.2024.100333","url":null,"abstract":"<div><p>Designer fuel fraud consists in the smuggling of modified diesel blends as engine lubricant oils and their illegal trade avoiding payment of the excise duty applied to energy products. The fraudulent mixture contains regular diesel fuel plus a heavier hydrocarbon fraction, originating from waste automotive lubricant or cheap, residual base oils.</p><p>Raman spectroscopy was tested as a rapid <em>in-situ</em> screening method to separate regular diesel fuel samples from those suspected to contain a heavier component, and thus demanding a more extensive characterization. The Raman fingerprint region from the screened sample is matched to purposely created spectral libraries of compliant and non-compliant diesel fuels using the instrumental search algorithm. Overall, 177 compliant fuel samples and 28 non-compliant samples (all designer fuels with a confirmed heavier fraction and/or anomalous distillation parameters) were measured. The designer fuels were all positively identified, with ∼18 % false positives.</p><p>Subsequently, the Raman data-set was studied by Principal Component Analysis (PCA) and then classified as either compliant or non-compliant using Linear Discriminant Analysis (LDA). PCA using up to three principal components for data visualization shows only an incipient separation but still a partial overlap between compliant and non-compliant samples. LDA, on the opposite, performed superiorly in the binary classification task, with no false negatives and less than 4 % false positives.</p></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S266683192400047X/pdfft?md5=36a6cce6e9cff39c951ac371aa1fbf70&pid=1-s2.0-S266683192400047X-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141142722","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A novel cannabinoid in hemp: Isolation by flash chromatography and identification by liquid chromatography high resolution mass spectrometry 大麻中的一种新型大麻素:闪蒸色谱法分离和液相色谱高分辨质谱法鉴定
Q3 Chemistry Pub Date : 2024-05-22 DOI: 10.1016/j.talo.2024.100332
Imma Ferrer, E.Michael Thurman

A novel and major cannabinoid (epicannabidiol hydrate) present in hemp plants and oils was isolated and characterized by a combination of flash chromatography and liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC/Q-TOF-MS). This novel cannabinoid differs from cannabidiol (CBD) by the absence of a double bond in the terpene ring and the presence of an additional hydroxyl group in the same terpene ring. The isolation procedure involved the use of normal phase chromatography with a silica gel preparative column, followed by reversed phase chromatography with a C18 preparative column. In this way, other major cannabinoids present in the samples, such as cannabidiol and Δ9-tetrahydrocannabinol, were separated and the focus was placed on the novel cannabinoid compound. Exact accurate masses were obtained for the compound of interest at m/z = 333.2424 in positive ion mode and m/z = 331.2279 in negative ion mode. Additional MS-MS analysis in negative ion mode revealed the position of the additional hydroxyl group in the molecule. Finally, the structural characterization was corroborated with 1H NMR and 13C NMR analysis, thus verifying the exact chemical structure of this novel cannabinoid, which has not previously been reported in hemp samples.

通过结合使用闪蒸色谱法和液相色谱法以及四极杆飞行时间质谱法(LC/Q-TOF-MS),对大麻植物和大麻油中的一种新型主要大麻素(表大麻二酚水合物)进行了分离和表征。这种新型大麻素与大麻二酚(CBD)的不同之处在于萜烯环中没有双键,而在同一萜烯环中存在一个额外的羟基。分离程序包括使用硅胶制备柱进行正相色谱分析,然后使用 C18 制备柱进行反相色谱分析。通过这种方法,样品中的其他主要大麻素(如大麻二酚和Δ9-四氢大麻酚)被分离出来,重点放在了新型大麻素化合物上。相关化合物在正离子模式下的精确质量为 m/z = 333.2424,在负离子模式下的精确质量为 m/z = 331.2279。在负离子模式下进行的其他 MS-MS 分析显示了分子中额外羟基的位置。最后,通过 1H NMR 和 13C NMR 分析证实了结构特征,从而验证了这种新型大麻素的确切化学结构,此前从未有大麻样本中含有这种物质的报道。
{"title":"A novel cannabinoid in hemp: Isolation by flash chromatography and identification by liquid chromatography high resolution mass spectrometry","authors":"Imma Ferrer,&nbsp;E.Michael Thurman","doi":"10.1016/j.talo.2024.100332","DOIUrl":"10.1016/j.talo.2024.100332","url":null,"abstract":"<div><p>A novel and major cannabinoid (epicannabidiol hydrate) present in hemp plants and oils was isolated and characterized by a combination of flash chromatography and liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (LC/Q-TOF-MS). This novel cannabinoid differs from cannabidiol (CBD) by the absence of a double bond in the terpene ring and the presence of an additional hydroxyl group in the same terpene ring. The isolation procedure involved the use of normal phase chromatography with a silica gel preparative column, followed by reversed phase chromatography with a C18 preparative column. In this way, other major cannabinoids present in the samples, such as cannabidiol and Δ9-tetrahydrocannabinol, were separated and the focus was placed on the novel cannabinoid compound. Exact accurate masses were obtained for the compound of interest at <em>m/z</em> = 333.2424 in positive ion mode and <em>m/z</em> = 331.2279 in negative ion mode. Additional MS-MS analysis in negative ion mode revealed the position of the additional hydroxyl group in the molecule. Finally, the structural characterization was corroborated with <sup>1</sup>H NMR and <sup>13</sup>C NMR analysis, thus verifying the exact chemical structure of this novel cannabinoid, which has not previously been reported in hemp samples.</p></div>","PeriodicalId":436,"journal":{"name":"Talanta Open","volume":null,"pages":null},"PeriodicalIF":0.0,"publicationDate":"2024-05-22","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.sciencedirect.com/science/article/pii/S2666831924000468/pdfft?md5=7213e08c76d4c10d40595c0ef35eb26d&pid=1-s2.0-S2666831924000468-main.pdf","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"141130244","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
期刊
Talanta Open
全部 Acc. Chem. Res. ACS Applied Bio Materials ACS Appl. Electron. Mater. ACS Appl. Energy Mater. ACS Appl. Mater. Interfaces ACS Appl. Nano Mater. ACS Appl. Polym. Mater. ACS BIOMATER-SCI ENG ACS Catal. ACS Cent. Sci. ACS Chem. Biol. ACS Chemical Health & Safety ACS Chem. Neurosci. ACS Comb. Sci. ACS Earth Space Chem. ACS Energy Lett. ACS Infect. Dis. ACS Macro Lett. ACS Mater. Lett. ACS Med. Chem. Lett. ACS Nano ACS Omega ACS Photonics ACS Sens. ACS Sustainable Chem. Eng. ACS Synth. Biol. Anal. Chem. BIOCHEMISTRY-US Bioconjugate Chem. BIOMACROMOLECULES Chem. Res. Toxicol. Chem. Rev. Chem. Mater. CRYST GROWTH DES ENERG FUEL Environ. Sci. Technol. Environ. Sci. Technol. Lett. Eur. J. Inorg. Chem. IND ENG CHEM RES Inorg. Chem. J. Agric. Food. Chem. J. Chem. Eng. Data J. Chem. Educ. J. Chem. Inf. Model. J. Chem. Theory Comput. J. Med. Chem. J. Nat. Prod. J PROTEOME RES J. Am. Chem. Soc. LANGMUIR MACROMOLECULES Mol. Pharmaceutics Nano Lett. Org. Lett. ORG PROCESS RES DEV ORGANOMETALLICS J. Org. Chem. J. Phys. Chem. J. Phys. Chem. A J. Phys. Chem. B J. Phys. Chem. C J. Phys. Chem. Lett. Analyst Anal. Methods Biomater. Sci. Catal. Sci. Technol. Chem. Commun. Chem. Soc. Rev. CHEM EDUC RES PRACT CRYSTENGCOMM Dalton Trans. Energy Environ. Sci. ENVIRON SCI-NANO ENVIRON SCI-PROC IMP ENVIRON SCI-WAT RES Faraday Discuss. Food Funct. Green Chem. Inorg. Chem. Front. Integr. Biol. J. Anal. At. Spectrom. J. Mater. Chem. A J. Mater. Chem. B J. Mater. Chem. C Lab Chip Mater. Chem. Front. Mater. Horiz. MEDCHEMCOMM Metallomics Mol. Biosyst. Mol. Syst. Des. Eng. Nanoscale Nanoscale Horiz. Nat. Prod. Rep. New J. Chem. Org. Biomol. Chem. Org. Chem. Front. PHOTOCH PHOTOBIO SCI PCCP Polym. Chem.
×
引用
GB/T 7714-2015
复制
MLA
复制
APA
复制
导出至
BibTeX EndNote RefMan NoteFirst NoteExpress
×
0
微信
客服QQ
Book学术公众号 扫码关注我们
反馈
×
意见反馈
请填写您的意见或建议
请填写您的手机或邮箱
×
提示
您的信息不完整,为了账户安全,请先补充。
现在去补充
×
提示
您因"违规操作"
具体请查看互助需知
我知道了
×
提示
现在去查看 取消
Book学术官方微信
Book学术文献互助
Book学术文献互助群
群 号:481959085
Book学术
文献互助 智能选刊 最新文献 互助须知 联系我们:info@booksci.cn
Book学术提供免费学术资源搜索服务,方便国内外学者检索中英文文献。致力于提供最便捷和优质的服务体验。
Copyright © 2023 Book学术 All rights reserved.
ghs 京公网安备 11010802042870号 京ICP备2023020795号-1