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Professor Susanne Rath, a researcher who has bravely faced challenges since childhood, kindly granted BrJAC an interview Susanne Rath教授,一个从小勇敢面对挑战的研究员,好心地给了BrJAC一个采访机会
IF 0.7 Q4 Chemistry Pub Date : 2022-10-05 DOI: 10.30744/brjac.2179-3425.interview.srath
S. Rath
Susanne Rath is an associate professor in the Institute of Chemistry at the University of Campinas (Unicamp), where she coordinates the “Laboratório de Bioanalítica Paracelsus”. She graduated with a Bachelor's degree in Chemistry (1983) from the University of Brasília (UnB), a Master’s degree in Chemistry (1986) from Unicamp, and a Ph.D in Pharmaceutical Chemistry (1990) from the Johann Wolfgang Goethe Universität Frankfurt am Main, Germany. So far, she has published 110 articles and seven book chapters, had four patents granted, and she has presented over 230 papers at scientific conferences. She supervised 17 master's students, 20 doctorate students and 10 post-docs. In addition, she coordinated 23 research projects supported by Brazilian funding agencies. Prof. Dr. Rath’s primary research is focused on toxic compounds in food, residue depletion studies of veterinary drugs in food-producing animals, development and validation of analytical methods, application of bidimensional chromatography and mass spectrometry, environmental impact assessment of veterinary drugs, antimicrobial resistance and N-nitrosamines in food, cosmetics and drugs. Since 2007, Prof. Rath has been a member of the Joint Expert Committee on Food Additives (JECFA) of the Food and Agriculture Organization of the United Nations (FAO) and the World Health Organization (WHO). Since 2011, Prof. Rath has been a member of the Technical Group on Maximum Residue Limits for Veterinary Drugs in Food of the National Health Surveillance Agency (Anvisa) of the Ministry of Health of Brazil.
Susanne Rath是坎皮纳斯大学(Unicamp)化学研究所的副教授,负责协调“Laboratório de Bioanalítica Paracelsus”项目。她毕业于University of Brasília (UnB)的化学学士学位(1983年),Unicamp的化学硕士学位(1986年),以及德国法兰克福的Johann Wolfgang Goethe Universität的药物化学博士学位(1990年)。到目前为止,她已经发表了110篇文章和7本书章节,获得了4项专利,并在科学会议上发表了230多篇论文。硕士生17人,博士生20人,博士后10人。此外,她还协调了23个由巴西资助机构支持的研究项目。Rath教授的主要研究领域包括食品中的有毒化合物、兽药在食用动物体内的残留去除研究、分析方法的开发和验证、二维色谱和质谱的应用、兽药的环境影响评估、抗微生物药物耐药性和食品、化妆品和药物中的n -亚硝胺。自2007年以来,Rath教授一直是联合国粮食及农业组织(粮农组织)和世界卫生组织(世卫组织)食品添加剂联合专家委员会(JECFA)的成员。自2011年以来,Rath教授一直是巴西卫生部国家卫生监督局(Anvisa)食品中兽药最大残留限量技术小组的成员。
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引用次数: 1
Paper-based microfluidics: What can we expect? 基于纸张的微流体:我们可以期待什么?
IF 0.7 Q4 Chemistry Pub Date : 2022-10-05 DOI: 10.30744/brjac.2179-3425.point-of-view-wktcoltro.n37
W. Coltro
In the last three decades, the scientific community has observed exponential growth in the development of microfluidic platforms and their use for applications in different fields. The noticeable advances are attributed to the advantages provided by miniaturization.1 In summary, the downscaling of analytical devices has offered attractive features, including reduced consumption of samples and reagents, short analysis time, and minimal waste generation. In addition, the possibility to perform multiplexed assays in portable devices without bulky instrumentation is another attractive feature that boosted the investigation of miniaturized devices with the capability to be tested directly in the point-of-care (POC). Due to the sample volume required to proceed with a chemical analysis on a microscale (typically in the µL range), a complete understanding of the fluid control and handle on channels defined in micrometric dimensions was necessary, giving rise to the science known as microfluidics.2 Many platforms including rigid and flexible materials can be explored for manufacturing microfluidic networks. Among all the substrates reported in the literature, the “paper” is by far the simplest and cheapest material currently employed for the development of microfluidic devices dedicated to analytical, bioanalytical, biomedical, environmental, food, and forensics applications.3 For many readers, the first question is why paper is used instead of other materials such as glass. Well, glass is a rigid material, and microchannel engraving requires cleanroom facilities, photolithographic patterning, developing steps, and thermal sealing. This standard protocol makes use of sophisticated instrumentation, and it is not readily available to most researchers. In this way, paper emerges as a simple and alternative material to be used for microfluidics. One of the major benefits of microfluidics refers to the sample-in-answer-out capability, which requires a fully automated fluid control to allow sample preparation, analytical separation, and detection stages. The fluid-controlled handling inside microchannels opens the possibility to integrate multiple analytical tasks in parallel into a high-throughput device. Considering these possibilities, it is worthwhile reflecting on how paper can be used to transport and handle a fluid. Paper is currently one of the most widely used raw materials in research laboratories. Its use has been explored for over a century. In 1949, a paper containing barriers made of paraffin was exploited to successfully demonstrate the elution of pigments within a channel based on the sample diffusion process.4 In 2007, paper was reinvented by the Whitesides group as a globally affordable substrate material for the development of miniaturized analytical platforms.5 Since this period, paper has become an increasingly popular platform for multipurpose applications. Probably, its broad use is associated with advantages over other conventional subs
基于纸张的微流体设备,包括简单点测试阵列、化学传感器、生物传感器、电化学传感器、可穿戴设备和侧流分析的例子,已在与分析和生物分析化学相关的主要科学期刊上找到。7-10在该院,在最近的文献中看到的大多数进展已经证明了在耐用性、保质期、再现性、稳健性和分析可靠性方面的改进,这使得基于纸张的微流体设备成为有希望和新兴的候选者,可以作为其他材料的替代品在市场上获得空间。通过这种方式,创业和创新值得强调,并成为许多有兴趣开设企业或公司的研究人员关注的焦点。学院和生产部门之间的桥梁取决于投资和参与,以克服行政和法律官僚机构,不仅是为了开办一家公司,而且是为了保持公司的全面运营模式。微流体装置的商业化一直在不断发展。例如,在过去三年中,位于不同国家的许多公司每年的出货量超过5亿台,清楚地表明了微流体设备在不同应用领域的潜力,包括药物输送、流动化学、分析设备、制药和生命科学,护理点诊断以及临床和兽医设置。11考虑到纸质材料的优势,我们在未来几年可以期待什么?市场上越来越多地希望能找到具有样本输入-应答功能的商用产品。由于纸张在全球范围内的可负担性,以及其在创建微流体和传感器原型方面的吸引力,有可能看到一个充满成功可能性的真正利基市场。从这个角度来看,现在是时候尽最大努力,生产可穿戴传感器或侧流设备等商用纸基产品,以监测血液、尿液、血清、汗液、唾液和眼泪等不同生物流体中的临床相关化合物了。独立或与知名公司合作的分拆或创业可能会加速这一进程。换句话说,现在是时候创新并将一个想法转化为具有社会影响的商业产品了。快速测试和最终用户直接做出的即时响应之间的接口是市场和风险分析中非常理想的功能。严重急性呼吸系统综合征冠状病毒2型在全球范围内的爆发是最新的例子,科学可以在几分钟内提供获得临床诊断的可能性,让人们能够决定理想的治疗方法,或者在这种情况下,进行社会隔离以防止病毒传播。数十种基于严重急性呼吸系统综合征冠状病毒2型纸条的自我诊断试剂盒已经在药店、医院或医疗诊所商业化。类似的策略可能很快就会出现在猴痘或其他全球疫情中。
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引用次数: 0
In Memoriam - BrJAC mourns the death of Prof. Dr. Carol Hollingworth Collins and recognizes her great contribution to the Analytical Chemistry in Brazil 纪念- BrJAC哀悼Carol Hollingworth Collins教授的去世,并认可她对巴西分析化学的巨大贡献
IF 0.7 Q4 Chemistry Pub Date : 2022-10-05 DOI: 10.30744/brjac.2179-3425.inmemoriam.carol-collins
C. Bottoli
Professor Carol Collins graduated in Chemistry from Bates College (1952) and obtained her PhD in Organic Physical Chemistry from Iowa State University of Science and Technology (1958), when she was introduced to the recently developed gas–liquid chromatography. She conducted postdoctoral research at the University of Wisconsin and later worked on radiochemistry and nuclear medicine at the Brookhaven National Laboratory and the Western New York Nuclear Research Center in Louvain (Belgium) and Southwest Asia. Professor Collins came to the State University of Campinas (Unicamp) with her husband, Kenneth Collins, in July 1974, during the university’s first decade, and played a leading role in consolidation of the Institute of Chemistry at Unicamp and in the growth of chemistry and analytical chemistry in Brazil. Her first line of research in Brazil was radioanalytical chemistry, later focusing on chromatographic techniques, initially applied to the products of radiochemical reactions and radiation chemistry. Subsequently, her attention was directed to the preparation of stationary phases for liquid chromatography. She gained remarkable achievement in the area of chromatography that allowed her to publish two books that are very popular in Brazil: "Introduction to Chromatographic Methods" (1987) and "Fundamentals of Chromatography" (2006). Her scientific and technological contributions have been recognized through several awards, including the “Marie Curie Award” from the American Association of University Women and the “Simão Mathias Medal” from the Brazilian Chemical Society (SBQ). She also received honors in recognition of the contributions of Unicamp's 40th anniversary, SBQ's 30th anniversary, a tribute from the Journal of the Brazilian Chemical Society, the National Meeting of Analytical Chemistry, the School of Separations and the Brazilian Symposium on Chromatography and Related Techniques (SIMCRO) Medal. For her outstanding performance and leadership in the creation and consolidation of the Analytical Chemistry Division of the Brazilian Chemical Society, her name was recognized in the Carol Collins Medal given to each National Meeting of Analytical Chemistry since the 2018 edition. Professor Collins was also a full member of the Brazilian Academy of Sciences and the Academy of Sciences of São Paulo, and received the title of Professor Emerita of Unicamp on 14 May 2012, in addition to being Emeritus Researcher at the National Council for Scientific and Technological Development (CNPq). Apart from her scientific competence, some characteristics shaped her personality and made her very popular among her colleagues and students: her vast gourmet knowledge, keen taste for caipirinha and coffee, infallible memory, great love for her work and for Brazil, dedication to science, analytical chemistry/chromatography, kindness as a person and her incessant search for justice. She was always receptive to clarifying the doubts of students, teachers and inte
Carol Collins教授1952年毕业于贝茨学院化学专业,1958年在爱荷华州立科技大学获得有机物理化学博士学位,当时她接触了最近发展起来的气液色谱法。她在威斯康星大学进行博士后研究,后来在布鲁克海文国家实验室和位于比利时鲁汶和西南亚的西纽约核研究中心从事放射化学和核医学工作。1974年7月,在坎皮纳斯州立大学(Unicamp)成立的第一个十年期间,柯林斯教授与丈夫肯尼斯·柯林斯(Kenneth Collins)来到坎皮纳斯州立大学(Unicamp),并在坎皮纳斯州立大学化学研究所的整合以及巴西化学和分析化学的发展中发挥了主导作用。她在巴西的第一个研究方向是放射分析化学,后来专注于色谱技术,最初应用于放射化学反应和辐射化学的产物。随后,她的注意力转向了液相色谱固定相的制备。她在色谱学领域取得了显著成就,出版了两本在巴西非常受欢迎的书:《色谱方法入门》(1987年)和《色谱学基础》(2006年)。她的科学和技术贡献获得了多个奖项的认可,包括美国大学妇女协会的“玛丽居里奖”和巴西化学学会(SBQ)的“sim o Mathias奖章”。她还获得了Unicamp成立40周年、SBQ成立30周年、巴西化学学会杂志、全国分析化学会议、分离学院和巴西色谱及相关技术研讨会(SIMCRO)奖章等荣誉。由于她在巴西化学会分析化学部门的创建和巩固方面的杰出表现和领导作用,自2018年以来,她的名字被授予每个国家分析化学会议的卡罗尔·柯林斯奖章。Collins教授还是巴西科学院和圣保罗科学院的正式成员,并于2012年5月14日获得Unicamp的荣誉教授头衔,此外他还是国家科学和技术发展委员会(CNPq)的荣誉研究员。除了她的科学能力之外,她的一些特点塑造了她的个性,并使她在同事和学生中非常受欢迎:她丰富的美食知识,对凯皮林纳酒和咖啡的敏锐品味,准确的记忆力,对她的工作和巴西的热爱,对科学的奉献,分析化学/色谱,为人善良,以及对正义的不断追求。她总是乐于澄清学生、老师和有关各方的疑问,她做得非常愉快,这是一个喜欢教授和传播知识的人的特点。柯林斯教授对人力资源培训、Unicamp化学研究所的巩固和发展以及巴西和国外分析化学/色谱部门的贡献是不可估量的。她辉煌的人生轨迹将留下难以估量的巨大遗产,她将永远留在那些有幸与她生活在一起的人的记忆中。
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引用次数: 0
Chemometrics reveals not-so-obvious analytical information 化学计量学揭示了不太明显的分析信息
IF 0.7 Q4 Chemistry Pub Date : 2022-10-05 DOI: 10.30744/brjac.2179-3425.letter-fabiolaverbi.n37
F. Pereira
The application of chemometric tools in analytical chemistry or other areas of chemistry has become essential. This is mainly due to the large amount and nature of the generated data1,2 and the need to extract useful information from these and optimize steps throughout a process. It allows the quick decision-making visualization of interactions among variables, such as synergism or antagonism between parameters, during the development of a method,3 as shown in Figure 1. Classical chemometric techniques have been disseminated and can be divided according to the study approach, among which exploratory data analysis stands out. Principal component analysis (PCA) is one of the most accessible and well-established ways to perform an initial exploration and extract relevant information from a given dataset and has been used quite successfully in various spectroscopic techniques.4 Principal component analysis consists of projecting the data in a smaller dimension, enabling the detection of anomalous samples (outliers), the selection of essential variables in a given system, and unsupervised classification.1,2,4 Another branch of chemometrics involves the design of experiments (DoE). The primary purpose of the factorial design is to study the influence or effect of a given variable and its interactions in a specific system.5-9 Multivariate calibration is another aspect of chemometrics, where several variables are used to calibrate one (or more) property or the concentration of a given chemical analyte.10,11 Since the first publications of chemometric tools, numerous variations of these techniques, proposals for data fusion strategies, and applications using hyphenated instrumental techniques have been proposed.12-14 Industrial quality control and development (R&D) laboratories require an approach addressing adequate quality by design (QbD). The QbD strategies consider four steps that include an analytical target profile (ATP), a risk assessment, a design space (DS), and control strategy and validation based on figures of merit, for instance.9 Principal component analysis is the most widely multivariate technique used for data analysis. Jolliffe wrote a review reporting his wonderful experience with PCA in the last 50 years.15 Indeed, PCA is an invaluable method for data, and I agree with it. PCA is the algorithm of choice for numerous chemometric techniques.16 Other computational languages, such as Python, are currently experiencing a rise in popularity in the field of chemistry. The R language has also become more popular than it was ten years ago. The scripts, functions, or codes are easily written with fewer lines and specific commands that minimize steps and help speed up calculations. The dissemination of free software has also become popular, and the sharing of codes through publications, social media, communities, or websites has become relatively easy. From my point of view, chemometrics is no longer faced as a giant monster or a way to become sc
化学计量工具在分析化学或其他化学领域的应用已经变得必不可少。这主要是由于生成的数据数量和性质都很大1,2,并且需要从这些数据中提取有用的信息并优化整个流程中的步骤。它允许在方法开发过程中对变量之间的交互进行快速决策可视化,例如参数之间的协同作用或对抗作用,如图1所示。经典的化学计量学技术已经广为传播,并可以根据研究方法进行划分,其中探索性数据分析是最突出的。主成分分析(PCA)是从给定数据集中进行初步探索和提取相关信息的最容易获得和最完善的方法之一,并已成功地用于各种光谱技术主成分分析包括在较小的维度上投射数据,能够检测异常样本(异常值),在给定系统中选择基本变量以及无监督分类。化学计量学的另一个分支涉及实验设计(DoE)。析因设计的主要目的是研究特定系统中给定变量的影响或效应及其相互作用。5-9多元校准是化学计量学的另一个方面,其中使用几个变量来校准一个(或多个)属性或给定化学分析物的浓度。10,11自从化学计量工具首次发表以来,已经提出了这些技术的许多变体,数据融合策略的建议,以及使用连字仪器技术的应用。12-14工业质量控制和开发(R&D)实验室需要一种方法来解决充分的质量设计(QbD)。QbD策略考虑四个步骤,包括分析目标概要(ATP)、风险评估、设计空间(DS)、控制策略和基于价值数字的验证主成分分析是应用最广泛的多变量数据分析技术。15 . Jolliffe写了一篇综述,报告了他在过去50年里使用PCA的美妙经历的确,PCA是处理数据的一种非常宝贵的方法,我同意这一点。PCA是许多化学计量学技术的首选算法其他计算语言,如Python,目前在化学领域也越来越受欢迎。R语言也比十年前更受欢迎。脚本、函数或代码可以用更少的行和特定的命令轻松编写,从而最小化步骤并帮助加快计算速度。自由软件的传播也变得流行起来,通过出版物、社会媒体、社区或网站共享代码也变得相对容易。从我的角度来看,化学计量学不再是一个巨大的怪物,也不再是一种没有有用内容的科学论文的花哨方式。化学计量学首先通过单变量评估或使用简单的图提取不容易可视化的信息。如今,成千上万的仪器数据可以提供重要的化学信息,我们必须利用它们来提出有意义的建议。事实上,QbD证明了这一点,因为工业4.0已经成为现实。
{"title":"Chemometrics reveals not-so-obvious analytical information","authors":"F. Pereira","doi":"10.30744/brjac.2179-3425.letter-fabiolaverbi.n37","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.letter-fabiolaverbi.n37","url":null,"abstract":"The application of chemometric tools in analytical chemistry or other areas of chemistry has become essential. This is mainly due to the large amount and nature of the generated data1,2 and the need to extract useful information from these and optimize steps throughout a process. It allows the quick decision-making visualization of interactions among variables, such as synergism or antagonism between parameters, during the development of a method,3 as shown in Figure 1. Classical chemometric techniques have been disseminated and can be divided according to the study approach, among which exploratory data analysis stands out. Principal component analysis (PCA) is one of the most accessible and well-established ways to perform an initial exploration and extract relevant information from a given dataset and has been used quite successfully in various spectroscopic techniques.4 Principal component analysis consists of projecting the data in a smaller dimension, enabling the detection of anomalous samples (outliers), the selection of essential variables in a given system, and unsupervised classification.1,2,4 Another branch of chemometrics involves the design of experiments (DoE). The primary purpose of the factorial design is to study the influence or effect of a given variable and its interactions in a specific system.5-9 Multivariate calibration is another aspect of chemometrics, where several variables are used to calibrate one (or more) property or the concentration of a given chemical analyte.10,11 Since the first publications of chemometric tools, numerous variations of these techniques, proposals for data fusion strategies, and applications using hyphenated instrumental techniques have been proposed.12-14 Industrial quality control and development (R&D) laboratories require an approach addressing adequate quality by design (QbD). The QbD strategies consider four steps that include an analytical target profile (ATP), a risk assessment, a design space (DS), and control strategy and validation based on figures of merit, for instance.9 Principal component analysis is the most widely multivariate technique used for data analysis. Jolliffe wrote a review reporting his wonderful experience with PCA in the last 50 years.15 Indeed, PCA is an invaluable method for data, and I agree with it. PCA is the algorithm of choice for numerous chemometric techniques.16 Other computational languages, such as Python, are currently experiencing a rise in popularity in the field of chemistry. The R language has also become more popular than it was ten years ago. The scripts, functions, or codes are easily written with fewer lines and specific commands that minimize steps and help speed up calculations. The dissemination of free software has also become popular, and the sharing of codes through publications, social media, communities, or websites has become relatively easy. From my point of view, chemometrics is no longer faced as a giant monster or a way to become sc","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-10-05","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"46525004","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
A New Spectrophotometric Method to Determinate Lead (II) Ion in Vegetables with 2-[(6-Methoxy-2-benzothiazolyl) azo]-4-methoxy phenol as a New Reagent 以2-[(6-甲氧基-2-苯并噻唑)偶氮]-4-甲氧基苯酚为新试剂分光光度法测定蔬菜中铅(II)离子
IF 0.7 Q4 Chemistry Pub Date : 2022-09-26 DOI: 10.30744/brjac.2179-3425.ar-50-2022
khadeejah alyasiri, F. Al-Zubaidi, Layla Mohammed
A new, sensitive, and accurate spectrophotometric method for determining lead (II) ion in vegetables samples, using laboratory prepared reagent (6-MBTAMP) is developed. The reagent and pb+2 complex characterization included infrared spectroscopy, ultraviolet-visible spectrophotometry, elemental analysis (CHN), energy dispersive X-ray spectroscopy (EDX), and nuclear magnetic resonance spectroscopy (1HNMR & 13CNMR) techniques. The method depends on the reaction of lead (II) with the 6-MBTAMP reagent in a neutral medium to form a green-red complex which showed a maximum absorbance at 670 nm. The optimum conditions such as pH of the medium, reagent volume, reagent concentration, and time effect were also investigated carefully. Limit of detection (LOD), limit of quantification (LOQ) and Sandell’s sensitivity were calculated to be 0.181 mg L-1, 0.604 mg L-1 and 0.03 µg cm-2 respectively. The proposed method obeyed Beer’s law at range of 0.6-10 mg L-1 and the recovery percentage of the vegetable samples ranged from 71% to 106.6%. The suggested spectrophotometric technique is proved to be simple, fast and sensitive for determination of Pb (II) ion in vegetables samples.
建立了一种灵敏、准确的分光光度法测定蔬菜样品中铅(II)离子的新方法。试剂和pb+2配合物的表征包括红外光谱、紫外可见分光光度法、元素分析(CHN)、能量色散x射线光谱(EDX)和核磁共振光谱(1HNMR和13CNMR)技术。该方法依靠铅(II)与6-MBTAMP试剂在中性介质中反应形成绿-红络合物,在670 nm处显示出最大吸光度。考察了培养基pH、试剂体积、试剂浓度、时间效应等最佳条件。检测限(LOD)、定量限(LOQ)和Sandell灵敏度分别为0.181 mg L-1、0.604 mg L-1和0.03µg cm-2。该方法在0.6 ~ 10 mg L-1范围内符合Beer定律,蔬菜样品的回收率为71% ~ 106.6%。该方法简便、快速、灵敏,可用于蔬菜样品中Pb (II)的测定。
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引用次数: 0
Mass Spectrometry Imaging for fungal interaction analysis: Classic versus Imprinting Methods 用于真菌相互作用分析的质谱成像:经典方法与印迹方法
IF 0.7 Q4 Chemistry Pub Date : 2022-09-26 DOI: 10.30744/brjac.2179-3425.ar-44-2022
Tallyta Teixeira, Jorge Rodrigues Neto, Elias Silva, A. Conceição, Felix Siqueira, P. Abdelnur
Fungi can produce many bioactive metabolites, which are enhanced when challenged in co-culture competition. For a better evaluation of these metabolites, Mass Spectrometry Imaging (MSI) can be used to provide complementary information about the metabolite spatial localization. However, some adaptations are required on available methodologies in MSI for applications in microorganisms, particularly on sample preparation, due to the characteristics of each type of cell that has to be analyzed. The imprinting method has been shown to be a robust method when applied to sample preparation, but to our knowledge it has never been tested for microbial MALDI-MSI. Herein we applied both Classic and Imprinting MALDI-MSI to compare and analyze metabolites produced by Aspergillus terreus (ATCC® 20542TM) and Pleurotus pulmonarius fungi. For the classic method, the fungi were inoculated for 8 days with PDA medium in a MALDI glass slide. For the imprinting method, fungi were also inoculated for 8 days in a MALDI glass slide and then transferred to a filter paper by manual pressure using a homemade apparatus. Samples were then dehydrated and submitted to HCCA matrix application by sublimation. The chemical images were acquired by MALDI-MSI, and the metabolites were identified by UHPLC-ESI-MS/MS. Twelve ions were detected by MALDI-MSI, using classic (m/z 210.54, 276.99, 307.45, 321.04, 329.70, 346.12, 351.12, 462.41 and 484.02) and imprinting (m/z 313.64, 379.66 and 404.36) methods. Some ions presented a higher intensity in the interaction zone between fungi areas, especially the ions m/z 329.70, 351.12 and 484.02. These ions may be related to metabolites involved in communication between microorganisms, because these fungi formed a mutualistic interaction. All ions were investigated by UHPLC-ESI-MS/MS, and two were identified: adenosine monophosphate (C10H14N5O7P, m/z 346.12, [M-H]-) visualized in the Classic Method, and rubrophen (C22H20O6, m/z 379.66, [M-H]-) visualized in the Imprinting Method. The metabolites from microorganisms are rarely reported in MS/MS databases, which explains the difficulty in the identification of these compounds. Our MSI analysis using the classic method provided a higher number of detected ions. However, both classic and imprinting methods resulted in a complementary information, leading to the detection of ions that were not previously observed on the classic approach. Despite of the challenges encountered on the sample preparation and metabolite identification, using both classic and imprinting MALDI-MSI for bioprospection of fungi metabolites is a promising approach on the analytical field of mass spectrometry which can be later used in biotechnological applications.
真菌可以产生许多生物活性代谢物,在共培养竞争中受到挑战时,这些代谢物会增强。为了更好地评估这些代谢物,质谱成像(MSI)可以用来提供代谢物空间定位的补充信息。然而,由于必须分析的每种类型的细胞的特性,需要对MSI中适用于微生物的现有方法进行一些调整,特别是在样品制备方面。印迹方法已被证明是一个稳健的方法,当应用于样品制备,但据我们所知,它从未测试过微生物MALDI-MSI。本文采用Classic和Imprinting MALDI-MSI对土曲霉(Aspergillus terreus, ATCC®20542TM)和肺侧耳菌(Pleurotus pulmonarius)真菌产生的代谢物进行比较和分析。经典方法是用PDA培养基在MALDI玻片上接种8天。印迹法是将真菌在MALDI玻片上接种8天,然后用自制仪器手动加压转移到滤纸上。然后将样品脱水,并通过升华提交到HCCA基质应用。化学图像采用MALDI-MSI获取,代谢物采用UHPLC-ESI-MS/MS鉴定。采用经典法(m/z 210.54、276.99、307.45、321.04、329.70、346.12、351.12、462.41和484.02)和印迹法(m/z 313.64、379.66和404.36)对12个离子进行了检测。部分离子在真菌区相互作用区表现出较高的强度,特别是m/z 329.70、351.12和484.02离子。这些离子可能与参与微生物间交流的代谢物有关,因为这些真菌形成了互惠的相互作用。采用UHPLC-ESI-MS/MS对所有离子进行分析,鉴定出经典法显示的单磷酸腺苷(C10H14N5O7P, m/z 346.12, [m - h]-)和印迹法显示的红霉素(C22H20O6, m/z 379.66, [m - h]-)。来自微生物的代谢物很少在MS/MS数据库中报道,这解释了鉴定这些化合物的困难。我们的MSI分析使用经典方法提供了更多的检测离子。然而,经典方法和印迹方法都产生了互补的信息,导致检测到以前在经典方法中未观察到的离子。尽管在样品制备和代谢物鉴定方面遇到了挑战,但使用经典和印迹MALDI-MSI进行真菌代谢物的生物检测在质谱分析领域是一种很有前途的方法,可用于生物技术应用。
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引用次数: 1
Employing Auto-Machine Learning Algorithms for Predicting the Cold Filter Plugging and Kinematic Viscosity at 40 ºC in Biodiesel Blends using Vibrational Spectroscopy Data 采用自动机器学习算法利用振动光谱数据预测生物柴油混合物在40ºC下的冷滤器堵塞和运动粘度
IF 0.7 Q4 Chemistry Pub Date : 2022-08-31 DOI: 10.30744/brjac.2179-3425.ar-30-2022
A. Luna, A. Torres, Camilla L Cunha, I. Lima, Luis Nonato
This work aims to develop an auto-machine learning method using Mid-Infrared (MIR) spectroscopy data to determine the cold filter plugging point (CFPP) and kinematic viscosity at 40 ºC of biodiesel, diesel, and mixtures samples. The biodiesel was obtained by the transesterification reaction and later purified. The first dataset was composed of 108 blends (biodiesel obtained from different biomass such as soy, corn, sunflower, and canola) with binary, ternary and quaternary mixtures. The second dataset was composed of 227 blends of diesel-biodiesel and diesel-biodiesel-ethanol, respectively. The physical properties of the samples were obtained according to ABNT NBR 14747 and ABNT NBR 10441, respectively. The MIR Spectroscopy data were acquired from 7,800 to 450 cm-1, with a 4 cm-1 resolution and 20 scans. The spectra' baseline alignment was carried out using the asymmetric least squares method. A Savitzky–Golay filter was applied to a set of digital data points to smooth the data. This work used a first-order polynomial and a zero derivative function to smooth the spectra. The dataset was split into training and test sets using the function CreateDataPartition from the caret package. It was adopted 70% for training and 30% for test sets. In this work, the model training process was carried out using the open-source Python library LazyPredict. The LazyPredict returns the trained models and their performance metrics. The kinematic viscosity at 40 ºC of the biodiesel samples and their blends could be modeled using the MIR Spectroscopy dataset using different auto-machine learning algorithms. The RMSEP (Root Mean Square Error of Prediction) (≤ 0.02 mm2 s-1) was similar to the experimental error obtained after log transformation. The CFPP of the biodiesel samples and their blends could be modeled using the MIR Spectroscopy dataset by different auto-machine learning algorithms with an RMSEP (≤ 1.6 ºC) similar to the experimental error obtained by traditional methodology. Based on the lower computational time and the same performance observed by the RMSEP and R2 (coefficient of determination) values from different algorithms, it is recommended to use Ridge or Ridge Cross-Validation Regression models for both physical properties using MIR Spectroscopy data.
这项工作旨在开发一种自动机器学习方法,使用中红外(MIR)光谱数据来确定生物柴油、柴油和混合物样品在40ºC下的冷滤器堵塞点(CFPP)和运动粘度。通过酯交换反应获得生物柴油,随后进行纯化。第一个数据集由108种混合物(从大豆、玉米、向日葵和油菜籽等不同生物质中获得的生物柴油)与二元、三元和四元混合物组成。第二个数据集分别由227种柴油生物柴油和柴油生物柴油乙醇混合物组成。样品的物理性能分别根据ABNT NBR 14747和ABNT NBR 10441获得。MIR光谱数据采集范围为7800至450 cm-1,分辨率为4 cm-1,扫描次数为20次。使用不对称最小二乘法对光谱进行基线比对。Savitzky–Golay滤波器被应用于一组数字数据点,以平滑数据。这项工作使用了一阶多项式和零导数函数来平滑光谱。使用插入符号包中的函数CreateDataPartition将数据集拆分为训练集和测试集。70%用于训练,30%用于测试集。在这项工作中,模型训练过程是使用开源Python库LazyPredict进行的。LazyPredict返回经过训练的模型及其性能指标。生物柴油样品及其混合物在40ºC下的运动粘度可以使用MIR光谱学数据集使用不同的自动机器学习算法进行建模。RMSEP(预测均方根误差)(≤0.02 mm2 s-1)与对数变换后获得的实验误差相似。生物柴油样品及其混合物的CFPP可以通过不同的自动机器学习算法使用MIR光谱数据集进行建模,RMSEP(≤1.6ºC)与传统方法获得的实验误差相似。基于较低的计算时间和不同算法的RMSEP和R2(决定系数)值观察到的相同性能,建议使用MIR光谱数据对两种物理性质使用岭或岭交叉验证回归模型。
{"title":"Employing Auto-Machine Learning Algorithms for Predicting the Cold Filter Plugging and Kinematic Viscosity at 40 ºC in Biodiesel Blends using Vibrational Spectroscopy Data","authors":"A. Luna, A. Torres, Camilla L Cunha, I. Lima, Luis Nonato","doi":"10.30744/brjac.2179-3425.ar-30-2022","DOIUrl":"https://doi.org/10.30744/brjac.2179-3425.ar-30-2022","url":null,"abstract":"This work aims to develop an auto-machine learning method using Mid-Infrared (MIR) spectroscopy data to determine the cold filter plugging point (CFPP) and kinematic viscosity at 40 ºC of biodiesel, diesel, and mixtures samples. The biodiesel was obtained by the transesterification reaction and later purified. The first dataset was composed of 108 blends (biodiesel obtained from different biomass such as soy, corn, sunflower, and canola) with binary, ternary and quaternary mixtures. The second dataset was composed of 227 blends of diesel-biodiesel and diesel-biodiesel-ethanol, respectively. The physical properties of the samples were obtained according to ABNT NBR 14747 and ABNT NBR 10441, respectively. The MIR Spectroscopy data were acquired from 7,800 to 450 cm-1, with a 4 cm-1 resolution and 20 scans. The spectra' baseline alignment was carried out using the asymmetric least squares method. A Savitzky–Golay filter was applied to a set of digital data points to smooth the data. This work used a first-order polynomial and a zero derivative function to smooth the spectra. The dataset was split into training and test sets using the function CreateDataPartition from the caret package. It was adopted 70% for training and 30% for test sets. In this work, the model training process was carried out using the open-source Python library LazyPredict. The LazyPredict returns the trained models and their performance metrics. The kinematic viscosity at 40 ºC of the biodiesel samples and their blends could be modeled using the MIR Spectroscopy dataset using different auto-machine learning algorithms. The RMSEP (Root Mean Square Error of Prediction) (≤ 0.02 mm2 s-1) was similar to the experimental error obtained after log transformation. The CFPP of the biodiesel samples and their blends could be modeled using the MIR Spectroscopy dataset by different auto-machine learning algorithms with an RMSEP (≤ 1.6 ºC) similar to the experimental error obtained by traditional methodology. Based on the lower computational time and the same performance observed by the RMSEP and R2 (coefficient of determination) values from different algorithms, it is recommended to use Ridge or Ridge Cross-Validation Regression models for both physical properties using MIR Spectroscopy data.","PeriodicalId":9115,"journal":{"name":"Brazilian Journal of Analytical Chemistry","volume":null,"pages":null},"PeriodicalIF":0.7,"publicationDate":"2022-08-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45706617","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
引用次数: 0
Development and Validation of a Simple Spectrophotometric Method for Quantitative Determination of Sodium Diclofenac in Modified-Release Tablets 简便分光光度法测定改性缓释片中双氯芬酸钠含量的建立与验证
IF 0.7 Q4 Chemistry Pub Date : 2022-08-31 DOI: 10.30744/brjac.2179-3425.ar-35-2022
Razan Alkassab, Yumen Hilal, Amin Swed
In this study, a rapid, simple, economical and accurate spectrophotometric process was developed for the determination of sodium diclofenac in modified release tablets using ethanol 96% as an available and non-toxic solvent. Sodium diclofenac standard solution was scanned under UV (200-400 nm) in a 1 cm quartz cell to determine the maximum absorption wavelength which was 285 nm. This method was validated in accordance with the requirements of the International Conference on Harmonization (ICH), where the calibration curve showed linearity in the studied concentration range (5-30 μg mL-1) with correlation coefficient R² = 0.9993. The relative standard deviation of the accuracy studies was within the acceptable range (<2%). This method also achieved an excellent recovery ratio (Mean recovery ± S.D. = 100.44% ± 0.81) with high sensitivity (limit of detection 1.10 μg mL-1 and quantitation limit of 3.34 μg mL-1). The developed process applied successfully to determine sodium diclofenac in four commercial pharmaceuticals products (A, B, C and D) marketed locally as modified-release tablets. The product C showed the highest assay value 106% and product B showed the lowest value 98%. Hence, we recommend using this method to quantitatively determine of sodium diclofenac in pharmaceutical dosage forms.
以96%乙醇为有效无毒溶剂,建立了一种快速、简便、经济、准确的分光光度法测定改性缓释片中双氯芬酸钠的方法。在1cm石英池中在UV(200-400nm)下扫描双氯芬酸钠标准溶液以确定285nm的最大吸收波长。该方法根据国际协调会议(ICH)的要求进行了验证,其中校准曲线在所研究的浓度范围(5-30μg mL-1)内显示出线性,相关系数R²=0.9993。准确度研究的相对标准偏差在可接受范围内(<2%)。该方法具有良好的回收率(平均回收率±S.D.=100.44%±0.81)和高灵敏度(检测限1.10μg mL-1,定量限3.34μg mL-)。所开发的方法成功地用于测定四种商业药品(A、B、C和D)中的双氯芬酸钠,这些药品在当地以改性释放片的形式销售。产品C显示出最高的测定值106%,而产品B显示出最低的测定值98%。因此,我们建议用该方法定量测定药物剂型中双氯芬酸钠的含量。
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引用次数: 0
Desorption Electrospray Ionization Imaging for Neurotransmitters Evaluation: A Potential Approach to Parkinson’s Disease Monitoring 解吸电喷雾电离成像用于神经递质评估:帕金森病监测的一种潜在方法
IF 0.7 Q4 Chemistry Pub Date : 2022-08-03 DOI: 10.30744/brjac.2179-3425.rv-42-2022
Lanaia Maciel, R. Martins, D. Gondim, João V A Oliveira, Julia Pereira, Gustavo Pereira, Leonardo Ferreira, A. Chaves, B. Vaz
Parkinson's disease (PD) is globally known as the most common movement disorder and the second most common neurodegenerative disease. The disease includes the symptoms of involuntary limb tremors, stiffness, or inflexibility of limbs and joints, among others. Due to this, scientific reports on analytical methodologies to evaluate the progression of neurodegenerative diseases are extremely necessary. Traditional methods include histochemical, immunohistochemical, and ligand-based approaches, however, these approaches still suffer from selectivity limitations of association, leading to a wrong evaluation. In this context, mass spectrometry imaging methods, such as desorption electrospray ionization (DESI), are potential approaches to visualize the distribution of biomarkers that can lead to the information on the progress of PD. This review aims to bring a discussion of some DESI methodologies reported in the literature for the assessment of neurotransmitters associated with PD.
帕金森病(PD)是全球公认的最常见的运动障碍和第二常见的神经退行性疾病。该病包括肢体不自主震颤、僵硬或四肢和关节不灵活等症状。因此,关于评估神经退行性疾病进展的分析方法的科学报告是非常必要的。传统的方法包括组织化学、免疫组织化学和基于配体的方法,然而,这些方法仍然受到选择性关联的限制,导致错误的评估。在这种情况下,质谱成像方法,如解吸电喷雾电离(DESI),是可视化生物标志物分布的潜在方法,可以导致PD进展的信息。这篇综述的目的是讨论一些DESI方法报道的文献评估与PD相关的神经递质。
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引用次数: 0
Comparison of Ultrasound-assisted Methods for Copper Determination in Bovine and Ovine Liver as Strategies for Food Surveillance and Animal Status Monitoring 超声辅助法测定牛和绵羊肝脏中铜含量作为食品监测和动物状态监测策略的比较
IF 0.7 Q4 Chemistry Pub Date : 2022-08-03 DOI: 10.30744/brjac.2179-3425.ar-38-2022
Fiorella Iaquinta, J. Santander, M. Pistón, I. Machado
Four methods for the efficient extraction of copper from bovine and ovine liver were optimized. Sample preparation consisted of extractions with dilute nitric acid or dilute tetramethyl ammonium hydroxide, assisted by an ultrasonic bath or an ultrasonic probe. Copper was determined by flame atomic absorption spectrometry. The experimental conditions were optimized using multivariate experiments. All methods were considered adequate for copper extraction, however, the two methods involving the probe turned out to be more efficient and faster, so they were selected for subsequent validation. Trueness was verified after the analysis of a certified reference material and the performance of a microwave-assisted extraction. Results were statistically equivalent, at the 95% significance level, to the values declared on the certificate. Precision (expressed as relative standard deviation) was better than 5% for all methods. Samples obtained from Uruguayan animals were analyzed. Obtained results agreed with previous results from sheep and cattle abroad. The proposed methods are simple alternatives for food surveillance and animal status monitoring, being straightforward and aligned with Green Chemistry principles, as it was demonstrated by performing the analytical Eco-Scale comprehensive approach. A discussion related to the particle size distribution obtained during the multivariate experiments was also included, to give some deeper insight into ultrasound effect on the biological tissue in different media. In addition, ultrasound-assisted extraction was compared to magnetic stirring to prove the effect of ultrasound.
优化了从牛和绵羊肝脏中高效提取铜的四种方法。样品制备包括用稀硝酸或稀氢氧化四甲基铵萃取,并辅以超声波浴或超声波探针。采用火焰原子吸收光谱法测定铜。采用多元实验对实验条件进行了优化。所有方法都被认为适合铜提取,然而,涉及探针的两种方法被证明更有效、更快,因此选择它们进行后续验证。在分析了经认证的参考材料和微波辅助提取的性能后,验证了真实性。结果在95%的显著性水平上与证书上声明的值具有统计学等效性。所有方法的精密度(以相对标准偏差表示)均优于5%。对从乌拉圭动物身上获得的样本进行了分析。获得的结果与国外绵羊和牛的先前结果一致。所提出的方法是食品监测和动物状态监测的简单替代方法,简单明了,符合绿色化学原则,正如通过执行分析生态规模综合方法所证明的那样。还包括与多变量实验中获得的粒径分布有关的讨论,以深入了解不同介质中超声对生物组织的影响。此外,将超声辅助提取与磁力搅拌进行了比较,以证明超声的效果。
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引用次数: 1
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Brazilian Journal of Analytical Chemistry
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