Pub Date : 2023-04-23DOI: 10.3390/analytica4020010
Florentin Weiss, C. Schaefer, S. Zimmermann, T. Märk, C. Mayhew
Here, we present proof of principle studies to demonstrate how the product ions associated with the ion mobility peaks obtained from a High Kinetic Energy-Ion Mobility Spectrometer (HiKE-IMS) measurement of a volatile can be identified using a Proton Transfer Reaction/Selective Reagent Ion-Time-of-Flight-Mass Spectrometer (PTR/SRI-ToF-MS) when operating both instruments at the same reduced electric field value and similar humidities. This identification of product ions improves our understanding of the ion chemistry occurring in the ion source region of a HiKE-IMS. The combination of the two analytical techniques is needed, because in the HiKE-IMS three reagent ions (NO+, H3O+ and O2+•) are present at the same time in high concentrations in the reaction region of the instrument for reduced electric fields of 100 Td and above. This means that even with a mass spectrometer coupled to the HiKE-IMS, the assignment of the product ions to a given reagent ion to a high level of confidence can be challenging. In this paper, we demonstrate an alternative approach using PTR/SRI-ToF-MS that allows separate investigations of the reactions of the reagent ions NO+, H3O+ and O2+•. In this study, we apply this approach to four nitrile containing organic compounds, namely acetonitrile, 2-furonitrile, benzonitrile and acrylonitrile. Both the HiKE-IMS and the PTR/SRI-ToF-MS instruments were operated at a commonly used reduced electric field strength of 120 Td and with gas flows at the same humidities.
{"title":"Revealing the Ion Chemistry Occurring in High Kinetic Energy-Ion Mobility Spectrometry: A Proof of Principle Study","authors":"Florentin Weiss, C. Schaefer, S. Zimmermann, T. Märk, C. Mayhew","doi":"10.3390/analytica4020010","DOIUrl":"https://doi.org/10.3390/analytica4020010","url":null,"abstract":"Here, we present proof of principle studies to demonstrate how the product ions associated with the ion mobility peaks obtained from a High Kinetic Energy-Ion Mobility Spectrometer (HiKE-IMS) measurement of a volatile can be identified using a Proton Transfer Reaction/Selective Reagent Ion-Time-of-Flight-Mass Spectrometer (PTR/SRI-ToF-MS) when operating both instruments at the same reduced electric field value and similar humidities. This identification of product ions improves our understanding of the ion chemistry occurring in the ion source region of a HiKE-IMS. The combination of the two analytical techniques is needed, because in the HiKE-IMS three reagent ions (NO+, H3O+ and O2+•) are present at the same time in high concentrations in the reaction region of the instrument for reduced electric fields of 100 Td and above. This means that even with a mass spectrometer coupled to the HiKE-IMS, the assignment of the product ions to a given reagent ion to a high level of confidence can be challenging. In this paper, we demonstrate an alternative approach using PTR/SRI-ToF-MS that allows separate investigations of the reactions of the reagent ions NO+, H3O+ and O2+•. In this study, we apply this approach to four nitrile containing organic compounds, namely acetonitrile, 2-furonitrile, benzonitrile and acrylonitrile. Both the HiKE-IMS and the PTR/SRI-ToF-MS instruments were operated at a commonly used reduced electric field strength of 120 Td and with gas flows at the same humidities.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"345 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-04-23","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76572395","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}
Pub Date : 2023-04-11DOI: 10.3390/analytica4020009
Na Li, Shimeng Chen, Jun Yang, Jun Song, Yongxin Song
Chlorine-containing disinfectants have been widely used all over the world to prevent COVID-19. However, little is known about the potential risk of chlorine-containing disinfectants in the marine environment. Phaeodactylum tricornutum (P. tricornutum) is a typical marine economic diatom, often used as an effective biomarker in ecotoxicology research. Here, the present study has investigated the effect of different effective chlorine concentrations on photosynthesis of P. tricornutum by chlorophyll fluorescence spectroscopy. Results have demonstrated that chlorine exposure promoted the chlorophyll fluorescence intensity at initial stage (24 h), suggesting that a large amount of energy is emitted in the form of fluorescence. However, the chlorophyll fluorescence intensity could not be detected under the high effective chlorine concentrations (6.7 × 10−3, 1.0 × 10−2, 1.3 × 10−2 and 1.7 × 10−2 mg L−1) after 48 h, indicating that the chlorine had high toxicity leading to the death of microalgae. In addition, the emission spectra of P. tricornutum were determined to contain two distinct fluorescence peaks representing the core antenna of photosystem II (685 nm) and the photosystem I complexes (710 nm) in the control group. The fluorescence emission peak value at 685 nm is significantly lower than the peak value at 710 nm in the control group, whereas chlorine treatments were opposite. It can be concluded that microalgae can regulate the distribution of excitation energy between the two photosystems to ensure that algae can utilize light energy. The result also found that the peak position of fluorescence emission spectra has a blue shift in all of NaClO treatments. The fluorescence intensity of microalgae excited at 467 nm was lower than that at 439 nm in chlorine treatments, illustrating chlorophyll b antenna was more easily damaged than chlorophyll a antenna. Our findings are providing new insights into the changing mechanism of chlorophyll fluorescence on P. tricornutum under chlorine stress and valuable data for risk assessment of marine environments.
{"title":"Impacts of Chlorine on the Change of Chlorophyll Fluorescence Spectrum to Phaeodactylum tricornutum","authors":"Na Li, Shimeng Chen, Jun Yang, Jun Song, Yongxin Song","doi":"10.3390/analytica4020009","DOIUrl":"https://doi.org/10.3390/analytica4020009","url":null,"abstract":"Chlorine-containing disinfectants have been widely used all over the world to prevent COVID-19. However, little is known about the potential risk of chlorine-containing disinfectants in the marine environment. Phaeodactylum tricornutum (P. tricornutum) is a typical marine economic diatom, often used as an effective biomarker in ecotoxicology research. Here, the present study has investigated the effect of different effective chlorine concentrations on photosynthesis of P. tricornutum by chlorophyll fluorescence spectroscopy. Results have demonstrated that chlorine exposure promoted the chlorophyll fluorescence intensity at initial stage (24 h), suggesting that a large amount of energy is emitted in the form of fluorescence. However, the chlorophyll fluorescence intensity could not be detected under the high effective chlorine concentrations (6.7 × 10−3, 1.0 × 10−2, 1.3 × 10−2 and 1.7 × 10−2 mg L−1) after 48 h, indicating that the chlorine had high toxicity leading to the death of microalgae. In addition, the emission spectra of P. tricornutum were determined to contain two distinct fluorescence peaks representing the core antenna of photosystem II (685 nm) and the photosystem I complexes (710 nm) in the control group. The fluorescence emission peak value at 685 nm is significantly lower than the peak value at 710 nm in the control group, whereas chlorine treatments were opposite. It can be concluded that microalgae can regulate the distribution of excitation energy between the two photosystems to ensure that algae can utilize light energy. The result also found that the peak position of fluorescence emission spectra has a blue shift in all of NaClO treatments. The fluorescence intensity of microalgae excited at 467 nm was lower than that at 439 nm in chlorine treatments, illustrating chlorophyll b antenna was more easily damaged than chlorophyll a antenna. Our findings are providing new insights into the changing mechanism of chlorophyll fluorescence on P. tricornutum under chlorine stress and valuable data for risk assessment of marine environments.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"40 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-04-11","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76497109","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}
Pub Date : 2023-03-31DOI: 10.3390/analytica4020008
Fernanda C O L Martins, Djenaine de Souza
This study describes the preparation and use of a dental amalgam electrode for the voltammetric determination of triazine-based pesticides ametryn, atrazine, and simazine in natural waters, using square wave voltammetry. The experimental and voltammetric parameters were previously optimized, and analytical curves were constructed to calculate analytical parameters. The detection limits presented values that were lower than the maximum limits of residues permitted in natural water by the Brazilian Environmental Agency, 100 µg L−1 (100 ppb), and around the values obtained using other electrodic surfaces or high-performance liquid chromatography, traditionally used in triazine levels determination. Furthermore, the recovery percentages in pure electrolyte and natural waters were around 100%, demonstrating that the methodology proposed is suitable for determining triazines contamination in natural water samples, based on an environmentally friendly procedure.
本研究描述了一种牙科汞合金电极的制备和使用，用于伏安法测定天然水中三嗪类农药阿特拉津、阿特拉津和西马辛。预先优化了实验参数和伏安参数，并构建了分析曲线来计算分析参数。检测限的值低于巴西环境局允许的天然水中残留的最大限值100 μ g L−1 (100 ppb)，并且接近使用其他电表面或高效液相色谱法(传统上用于三嗪水平测定)获得的值。此外，在纯电解质和天然水中的回收率约为100%，表明所提出的方法适用于确定天然水样中的三嗪污染，基于环保程序。
{"title":"New Approaches in Electroanalytical Determination of Triazines-Based Pesticides in Natural Waters","authors":"Fernanda C O L Martins, Djenaine de Souza","doi":"10.3390/analytica4020008","DOIUrl":"https://doi.org/10.3390/analytica4020008","url":null,"abstract":"This study describes the preparation and use of a dental amalgam electrode for the voltammetric determination of triazine-based pesticides ametryn, atrazine, and simazine in natural waters, using square wave voltammetry. The experimental and voltammetric parameters were previously optimized, and analytical curves were constructed to calculate analytical parameters. The detection limits presented values that were lower than the maximum limits of residues permitted in natural water by the Brazilian Environmental Agency, 100 µg L−1 (100 ppb), and around the values obtained using other electrodic surfaces or high-performance liquid chromatography, traditionally used in triazine levels determination. Furthermore, the recovery percentages in pure electrolyte and natural waters were around 100%, demonstrating that the methodology proposed is suitable for determining triazines contamination in natural water samples, based on an environmentally friendly procedure.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"25 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-03-31","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"90962458","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}
Pub Date : 2023-03-16DOI: 10.3390/analytica4010007
Imran Ali, Syed Dilshad Alam, R. Raja, S. Khan, Rushda Anjum, A. K. Jain, H. Aboul‐Enein, M. Locatelli
Among many diseases, allergy appears to be a serious problem for human beings. Various forms of allergic disorders make people tense, leading to some other health issues. Many medications, including nonracemic and racemic ones, are used to treat this problem. It is important to have exact analysis strategies just to see any medication side effects, plasma profiles, and working efficiency. Therefore, efforts are made to review simple and chiral HPLC methods for antiallergic drugs; HPLC is the best analytical technique. The highlights in this article include the world scenario, causes of allergy, the effect of allergy on the economy, the mechanism of allergy in humans, classes of antiallergic drugs, simple drugs, chiral drugs, analysis by HPLC, and the chiral recognition mechanism. Moreover, attempts are also made to highlight the management of allergies and future perspectives.
{"title":"Advances in Simple and Chiral-HPLC Methods for Antiallergic Drugs and Chiral Recognition Mechanism","authors":"Imran Ali, Syed Dilshad Alam, R. Raja, S. Khan, Rushda Anjum, A. K. Jain, H. Aboul‐Enein, M. Locatelli","doi":"10.3390/analytica4010007","DOIUrl":"https://doi.org/10.3390/analytica4010007","url":null,"abstract":"Among many diseases, allergy appears to be a serious problem for human beings. Various forms of allergic disorders make people tense, leading to some other health issues. Many medications, including nonracemic and racemic ones, are used to treat this problem. It is important to have exact analysis strategies just to see any medication side effects, plasma profiles, and working efficiency. Therefore, efforts are made to review simple and chiral HPLC methods for antiallergic drugs; HPLC is the best analytical technique. The highlights in this article include the world scenario, causes of allergy, the effect of allergy on the economy, the mechanism of allergy in humans, classes of antiallergic drugs, simple drugs, chiral drugs, analysis by HPLC, and the chiral recognition mechanism. Moreover, attempts are also made to highlight the management of allergies and future perspectives.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"8 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-03-16","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84577788","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}
Pub Date : 2023-03-03DOI: 10.3390/analytica4010006
Mahyara Markievicz Mancio Kus-Yamashita, Cristiane Bonaldi Cano, Vânia Claudia Barros Monteiro, R. M. Catarino
Human milk provides all the nutrients required by babies during the first six months of their life. Human milk lipids represent the main source of energy, contributing almost 50% of the total energy content. Additionally, fatty acids ensure the correct development of children in the prenatal, postnatal, and infant phases. Docosahexaenoic acid (DHA) is essential for visual and cognitive development, and its presence during childhood can affect long-term health. This study aimed to optimize and validate a methodology for the direct determination of DHA in human milk. We used 20 samples of human milk from lactating women living in the city of Itu, São Paulo, who attended Basic Health Units from September 2019 to September 2020, and a sample of certified reference material from the National Institute of Standards and Technology. The proposed methodology consists of a validated mixed transesterification process without prior lipid extraction, optimized by factorial design. This methodology can be successfully used in human milk samples as it is both precise and accurate. The values of DHA in the sampled milks were similar to those in European countries and lower than those in Asian countries due to diet.
{"title":"Human Milk: Fast Determination of Docosahexaenoic Acid (DHA)","authors":"Mahyara Markievicz Mancio Kus-Yamashita, Cristiane Bonaldi Cano, Vânia Claudia Barros Monteiro, R. M. Catarino","doi":"10.3390/analytica4010006","DOIUrl":"https://doi.org/10.3390/analytica4010006","url":null,"abstract":"Human milk provides all the nutrients required by babies during the first six months of their life. Human milk lipids represent the main source of energy, contributing almost 50% of the total energy content. Additionally, fatty acids ensure the correct development of children in the prenatal, postnatal, and infant phases. Docosahexaenoic acid (DHA) is essential for visual and cognitive development, and its presence during childhood can affect long-term health. This study aimed to optimize and validate a methodology for the direct determination of DHA in human milk. We used 20 samples of human milk from lactating women living in the city of Itu, São Paulo, who attended Basic Health Units from September 2019 to September 2020, and a sample of certified reference material from the National Institute of Standards and Technology. The proposed methodology consists of a validated mixed transesterification process without prior lipid extraction, optimized by factorial design. This methodology can be successfully used in human milk samples as it is both precise and accurate. The values of DHA in the sampled milks were similar to those in European countries and lower than those in Asian countries due to diet.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"332 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-03-03","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80552547","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}
Pub Date : 2023-02-08DOI: 10.3390/analytica4010005
Kostas Gkountanas, Ioanna Dagla, E. Gikas, A. Malenović, Y. Dotsikas
Chromatograms with overlapping peaks and a baseline rise or upset constitute a great challenge for analysts. Such a case regarding the analysis of bupropion hydrochloride and its 5 impurities in a tablet formulation was used as a model. A baseline correction technique for liquid chromatography coupled with diode array detection is described by using Rstudio. The asymmetry least squares (ALS) algorithm was used as implemented in the “baseline” package, with parameters lambda and p set to 4 and 0.05, respectively. Peak deconvolution and subsequent integration and area quantification were accomplished through Fytik software. Chromatographic data from the validation procedure were utilized to demonstrate the feasibility of the suggested method and whether this correction affects the outcome of the validation study. Finally, a robustness study was carried out in order to shed light on the factors that have a more significant influence on the baseline correction, showing the reliability of this procedure through random changes in its parameters.
{"title":"Baseline Correction for HPLC Chromatograms by Using Free Open-Source Software","authors":"Kostas Gkountanas, Ioanna Dagla, E. Gikas, A. Malenović, Y. Dotsikas","doi":"10.3390/analytica4010005","DOIUrl":"https://doi.org/10.3390/analytica4010005","url":null,"abstract":"Chromatograms with overlapping peaks and a baseline rise or upset constitute a great challenge for analysts. Such a case regarding the analysis of bupropion hydrochloride and its 5 impurities in a tablet formulation was used as a model. A baseline correction technique for liquid chromatography coupled with diode array detection is described by using Rstudio. The asymmetry least squares (ALS) algorithm was used as implemented in the “baseline” package, with parameters lambda and p set to 4 and 0.05, respectively. Peak deconvolution and subsequent integration and area quantification were accomplished through Fytik software. Chromatographic data from the validation procedure were utilized to demonstrate the feasibility of the suggested method and whether this correction affects the outcome of the validation study. Finally, a robustness study was carried out in order to shed light on the factors that have a more significant influence on the baseline correction, showing the reliability of this procedure through random changes in its parameters.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"4 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-02-08","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"79693099","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}
Pub Date : 2023-02-01DOI: 10.3390/analytica4010004
M. Sturm, Erika Myers, Dennis Schober, Anika Korzin, Katrin Schuhen
Fluorescent staining of microplastics as a detection method is consistently gaining importance in microplastics research, as it is fast, easy to use, and requires low technical effort. In this study, a complete procedure was developed, from sample collection to sample processing and detection, to measure microplastics with low cost and time requirements. The developed procedure was tested by measuring the microplastics in the effluent of a German wastewater treatment plant over a period of one year. The results show that the process is especially well suited to investigate temporal variations of microplastic contamination, which requires a large number of samples to be processed. Further, the precision and selectivity of the detection process could be improved by applying newly developed Nile red derivatives for fluorescent staining. A low budget modification of a microscope for fluorescent imaging is compared to a modification with precise optical bandpass filters. A script enabling automated microplastic detection and counting was developed, improving the accuracy and comparability of the process.
{"title":"Development of an Inexpensive and Comparable Microplastic Detection Method Using Fluorescent Staining with Novel Nile Red Derivatives","authors":"M. Sturm, Erika Myers, Dennis Schober, Anika Korzin, Katrin Schuhen","doi":"10.3390/analytica4010004","DOIUrl":"https://doi.org/10.3390/analytica4010004","url":null,"abstract":"Fluorescent staining of microplastics as a detection method is consistently gaining importance in microplastics research, as it is fast, easy to use, and requires low technical effort. In this study, a complete procedure was developed, from sample collection to sample processing and detection, to measure microplastics with low cost and time requirements. The developed procedure was tested by measuring the microplastics in the effluent of a German wastewater treatment plant over a period of one year. The results show that the process is especially well suited to investigate temporal variations of microplastic contamination, which requires a large number of samples to be processed. Further, the precision and selectivity of the detection process could be improved by applying newly developed Nile red derivatives for fluorescent staining. A low budget modification of a microscope for fluorescent imaging is compared to a modification with precise optical bandpass filters. A script enabling automated microplastic detection and counting was developed, improving the accuracy and comparability of the process.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"30 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-02-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88382324","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}
Pub Date : 2023-01-18DOI: 10.3390/analytica4010003
C. Navarathna, H. Pray, Prashan M. Rodrigo, B. Arwenyo, Cassidy McNeely, Henry Reynolds, Natalie Hampton, K. Lape, Katie Roman, Maddie Heath, Sean Stokes, S. R. Gunatilake, G. Ariunbold, F. Perez, R. Thirumalai, E. M. Hassan, Islam Elsayed, D. Mohan, Ashli Brown, Debra Moore, S. Reichley, M. Lawrence, T. Mlsna
Global plastic production and usage has increased annually for decades and microplastic pollutants (≤5 mm) are a growing concern. Microplastics in surface waters can adsorb and desorb harmful chemicals such as per- and polyfluoroalkyl substances (PFAS). Microplastics can accumulate across all tropic levels in the marine food web. The purpose of this research was to analyze the stomach and intestinal contents of stranded (Mississippi coast) bottlenose dolphins and sea turtles for the presence of microplastics and commonly found PFAS, PFOS, PFOA, and GenX. Gut contents were digested (10% KOH in 50% MeOH) and then analyzed for microplastics using pyrolysis gas chromatography-mass spectrometry (Pyro-GC-MS), Nile red microscopy, X-ray photo electron spectroscopy (XPS), and Raman spectroscopy. Digested sample filtrate was pre-concentrated using solid-phase extraction (SPE) before PFAS liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The PFOS extraction and analysis had 98.6% recovery when validated with certified pike‒perch fish reference material. The Nile red testing on most samples revealed the presence of microplastics (Table S1). The Pyro-GC-MS results from two samples confirmed the presence of the plasticizer acetamide. The Raman spectroscopy analysis indicated characteristic plastic peaks corresponding to polystyrene in one sample. PFOS (95.5 to 1,934.5 µg/kg) was detected in three dolphin stomach samples. This project is part of a long-term study with the goal of a better understanding of microplastics and PFAS environmental contamination and their impact on bottlenose dolphins and sea turtles.
{"title":"Microplastics and Per- and Polyfluoroalkyl Substances (PFAS) Analysis in Sea Turtles and Bottlenose Dolphins along Mississippi’s Coast","authors":"C. Navarathna, H. Pray, Prashan M. Rodrigo, B. Arwenyo, Cassidy McNeely, Henry Reynolds, Natalie Hampton, K. Lape, Katie Roman, Maddie Heath, Sean Stokes, S. R. Gunatilake, G. Ariunbold, F. Perez, R. Thirumalai, E. M. Hassan, Islam Elsayed, D. Mohan, Ashli Brown, Debra Moore, S. Reichley, M. Lawrence, T. Mlsna","doi":"10.3390/analytica4010003","DOIUrl":"https://doi.org/10.3390/analytica4010003","url":null,"abstract":"Global plastic production and usage has increased annually for decades and microplastic pollutants (≤5 mm) are a growing concern. Microplastics in surface waters can adsorb and desorb harmful chemicals such as per- and polyfluoroalkyl substances (PFAS). Microplastics can accumulate across all tropic levels in the marine food web. The purpose of this research was to analyze the stomach and intestinal contents of stranded (Mississippi coast) bottlenose dolphins and sea turtles for the presence of microplastics and commonly found PFAS, PFOS, PFOA, and GenX. Gut contents were digested (10% KOH in 50% MeOH) and then analyzed for microplastics using pyrolysis gas chromatography-mass spectrometry (Pyro-GC-MS), Nile red microscopy, X-ray photo electron spectroscopy (XPS), and Raman spectroscopy. Digested sample filtrate was pre-concentrated using solid-phase extraction (SPE) before PFAS liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis. The PFOS extraction and analysis had 98.6% recovery when validated with certified pike‒perch fish reference material. The Nile red testing on most samples revealed the presence of microplastics (Table S1). The Pyro-GC-MS results from two samples confirmed the presence of the plasticizer acetamide. The Raman spectroscopy analysis indicated characteristic plastic peaks corresponding to polystyrene in one sample. PFOS (95.5 to 1,934.5 µg/kg) was detected in three dolphin stomach samples. This project is part of a long-term study with the goal of a better understanding of microplastics and PFAS environmental contamination and their impact on bottlenose dolphins and sea turtles.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"469 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-01-18","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"76807700","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}
Pub Date : 2023-01-17DOI: 10.3390/analytica4010002
High-quality academic publishing is built on rigorous peer review [...]
高质量的学术出版建立在严格的同行评审的基础上[…]
{"title":"Acknowledgment to the Reviewers of Analytica in 2022","authors":"","doi":"10.3390/analytica4010002","DOIUrl":"https://doi.org/10.3390/analytica4010002","url":null,"abstract":"High-quality academic publishing is built on rigorous peer review [...]","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"4 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-01-17","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84072260","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}
Pub Date : 2023-01-04DOI: 10.3390/analytica4010001
Maged Kharouba, S. Mahmoud
Levetiracetam (LEV) is a broad spectrum antiseizure medication that is used in various seizure types. There is evidence that therapeutic drug monitoring (TDM) of LEV is of value in selected patient populations, therefore determination of LEV plasma concentrations is essential. Herein we developed and validated a simple, reproducible, and practical method for the quantification of LEV concentrations in human plasma samples using high performance liquid chromatography (HPLC). Plasma samples (0.3 mL) deproteinization was done using acetonitrile. HPLC chromatographic separation of plasma samples was accomplished by reversed phase C18 column. The mobile phase constituted water and acetonitrile (90:10, v/v) ran at flow rate of 1 mL/min. Signal acquisition was conducted at a wavelength of 192 nm. Calibration curves showed excellent linearity (Correlation coefficient r2 > 0.99) over a concentration range of 3–80 μg/mL. Both inter and intraday assay accuracy and precision were less than 8% (except for the lowest limit of quantification was within 20%). Elution time was 15 min. The developed method excluded the use of buffers and utilized small volumes of plasma samples with simple mobile phase composition. Therefore, our method could be practically applied to routine TDM.
{"title":"Development and Validation of a Simple HPLC-UV Assay Method for Determination of Levetiracetam Concentrations in Human Plasma","authors":"Maged Kharouba, S. Mahmoud","doi":"10.3390/analytica4010001","DOIUrl":"https://doi.org/10.3390/analytica4010001","url":null,"abstract":"Levetiracetam (LEV) is a broad spectrum antiseizure medication that is used in various seizure types. There is evidence that therapeutic drug monitoring (TDM) of LEV is of value in selected patient populations, therefore determination of LEV plasma concentrations is essential. Herein we developed and validated a simple, reproducible, and practical method for the quantification of LEV concentrations in human plasma samples using high performance liquid chromatography (HPLC). Plasma samples (0.3 mL) deproteinization was done using acetonitrile. HPLC chromatographic separation of plasma samples was accomplished by reversed phase C18 column. The mobile phase constituted water and acetonitrile (90:10, v/v) ran at flow rate of 1 mL/min. Signal acquisition was conducted at a wavelength of 192 nm. Calibration curves showed excellent linearity (Correlation coefficient r2 > 0.99) over a concentration range of 3–80 μg/mL. Both inter and intraday assay accuracy and precision were less than 8% (except for the lowest limit of quantification was within 20%). Elution time was 15 min. The developed method excluded the use of buffers and utilized small volumes of plasma samples with simple mobile phase composition. Therefore, our method could be practically applied to routine TDM.","PeriodicalId":7829,"journal":{"name":"Analytica","volume":"1 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2023-01-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"88933168","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}
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