V. G. Milagres, Maria José Nunes de Paiva, M. M. d'Auriol‐Souza, A. L. Larentis, I. C. Costa-Amaral, L. C. André
The risk assessment of benzene exposure can be performed based on the analysis of biomarkers in biological monitoring processes. S‐phenylmercapturic acid is a specific benzene biomarker, and its analysis challenges the sensitivity of several analytical methods. The present study aims to develop and standardize an analytic procedure to determine this biomarker through gas chromatography–mass spectrometry, based on different extraction methods, to increase the sensitivity and specificity of the studied analytical method. Liquid–liquid extraction, solid‐phase extraction, liquid‐phase microextraction, and low‐temperature partitioning extraction were tested. The last one was the selected extraction method, which was validated to ensure their quality and reliability. The method above has shown linear correlation to benzene concentrations ranging from 5 to 60 μg L−1 and presented detection and quantification limits of 0.95 and 3.18 μg L−1, respectively. Intra and inter‐assay accuracy recorded variation coefficients equal 3.63% and 8.67%, respectively. The mean accuracy value was 98.72%. This procedure presented linearity, accuracy, and detection and quantification limits within the range of interest adopted to assess occupational and environmental exposure to benzene based on biomonitoring processes.
{"title":"Comparison study on extraction techniques used to assess S‐phenylmercapturic acid as low benzene exposure biomarker based on gas chromatography coupled with mass spectrometry","authors":"V. G. Milagres, Maria José Nunes de Paiva, M. M. d'Auriol‐Souza, A. L. Larentis, I. C. Costa-Amaral, L. C. André","doi":"10.1002/sscp.202300031","DOIUrl":"https://doi.org/10.1002/sscp.202300031","url":null,"abstract":"The risk assessment of benzene exposure can be performed based on the analysis of biomarkers in biological monitoring processes. S‐phenylmercapturic acid is a specific benzene biomarker, and its analysis challenges the sensitivity of several analytical methods. The present study aims to develop and standardize an analytic procedure to determine this biomarker through gas chromatography–mass spectrometry, based on different extraction methods, to increase the sensitivity and specificity of the studied analytical method. Liquid–liquid extraction, solid‐phase extraction, liquid‐phase microextraction, and low‐temperature partitioning extraction were tested. The last one was the selected extraction method, which was validated to ensure their quality and reliability. The method above has shown linear correlation to benzene concentrations ranging from 5 to 60 μg L−1 and presented detection and quantification limits of 0.95 and 3.18 μg L−1, respectively. Intra and inter‐assay accuracy recorded variation coefficients equal 3.63% and 8.67%, respectively. The mean accuracy value was 98.72%. This procedure presented linearity, accuracy, and detection and quantification limits within the range of interest adopted to assess occupational and environmental exposure to benzene based on biomonitoring processes.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2023-08-13","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"45488356","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}
Caroline Fernandes Grecco, V. Tumas, J. Hallak, M. E. Queiroz
Alzheimer's disease (AD) is a neurodegenerative disorder characterized by an extracellular accumulation of amyloid beta peptides in the brain. The concentration of the amyloid beta peptides in cerebrospinal fluid (CSF) have been evaluated as potential biomarkers of AD for early diagnostic. In this work, an in‐tube solid‐phase microextraction (in‐tube SPME) coupled to UHPLC–MS/MS method was established to determine amyloid beta peptides in CSF samples from AD patients. A strong cation‐exchange (sulfopropyl methacrylate‐co‐ethylene glycol dimethacrylate) monolithic capillary was synthesized on the inner surface of a fused silica capillary and used as an extractive phase for in‐tube SPME. The morphology and chemical structure of the monolithic phase were characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. The proposed method presented linear range from the lower limits of quantification 0.6 and 0.8 to 10 ng mL−1. Excluding the lower limits of quantification values, the analytical validation showed precision with the coefficient of variation values lower than 13.1%, and accuracy with relative standard deviation lower than 13.5%. The in‐tube SPME coupled to UHPLC–MS/MS method was successfully applied to determine amyloid beta peptides in CSF samples from AD patients.
{"title":"In‐tube solid‐phase microextraction (sulfopropyl methacrylate‐co‐ethylene glycol dimethacrylate monolithic capillary) coupled to LC–MS/MS to determine beta amyloid peptides in Alzheimer's cerebrospinal fluid samples","authors":"Caroline Fernandes Grecco, V. Tumas, J. Hallak, M. E. Queiroz","doi":"10.1002/sscp.202300044","DOIUrl":"https://doi.org/10.1002/sscp.202300044","url":null,"abstract":"Alzheimer's disease (AD) is a neurodegenerative disorder characterized by an extracellular accumulation of amyloid beta peptides in the brain. The concentration of the amyloid beta peptides in cerebrospinal fluid (CSF) have been evaluated as potential biomarkers of AD for early diagnostic. In this work, an in‐tube solid‐phase microextraction (in‐tube SPME) coupled to UHPLC–MS/MS method was established to determine amyloid beta peptides in CSF samples from AD patients. A strong cation‐exchange (sulfopropyl methacrylate‐co‐ethylene glycol dimethacrylate) monolithic capillary was synthesized on the inner surface of a fused silica capillary and used as an extractive phase for in‐tube SPME. The morphology and chemical structure of the monolithic phase were characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. The proposed method presented linear range from the lower limits of quantification 0.6 and 0.8 to 10 ng mL−1. Excluding the lower limits of quantification values, the analytical validation showed precision with the coefficient of variation values lower than 13.1%, and accuracy with relative standard deviation lower than 13.5%. The in‐tube SPME coupled to UHPLC–MS/MS method was successfully applied to determine amyloid beta peptides in CSF samples from AD patients.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2023-08-07","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"43610037","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}
Rutvik H Pandya, Hetaben M. Kachhiya, Dhavalsinh P. Solanki, Jinal N. Tandel, U. Chhalotiya, D. Shah
Anemia with chronic kidney disease treating newer hope is recently approved Desidustat. By following International Conference on Harmonization Quality guideline Q2 (R1), an economic high‐performance thin‐layer chromatography method has been developed for the estimation of Desidustat. Pre‐coated silica gel 60 F254 plates as stationary phase along with mobile phase toluene:methanol:glacial acetic acid (7.5:2.5:0.3 v/v/v), and 230 nm detection wavelength was selected as optimized. Developed method was found linear in quantity per band range of 100 ng/band to 600 ng/band for Desidustat with 0.9979 regression coefficient. Standard spiking method showed method accuracy with a mean percentage recovery of 99.21%–101.63%. Limit of detection and limit of quantitation were found to be 3.94 and 11.94 ng/band, respectively. The method was found to be linear, precise, accurate, robust, rugged, selective, sensitive, and specific for the quantification of Desidustat in bulk and tablet dosage form and successfully can be applied for the qualitative and quantitative determination of Desidustat in bulk and marketed tablet formulation.
{"title":"A sensitive, precise, accurate, and economic planar chromatographic method developed and validated for quantification of Desidustat as per guideline","authors":"Rutvik H Pandya, Hetaben M. Kachhiya, Dhavalsinh P. Solanki, Jinal N. Tandel, U. Chhalotiya, D. Shah","doi":"10.1002/sscp.202300069","DOIUrl":"https://doi.org/10.1002/sscp.202300069","url":null,"abstract":"Anemia with chronic kidney disease treating newer hope is recently approved Desidustat. By following International Conference on Harmonization Quality guideline Q2 (R1), an economic high‐performance thin‐layer chromatography method has been developed for the estimation of Desidustat. Pre‐coated silica gel 60 F254 plates as stationary phase along with mobile phase toluene:methanol:glacial acetic acid (7.5:2.5:0.3 v/v/v), and 230 nm detection wavelength was selected as optimized. Developed method was found linear in quantity per band range of 100 ng/band to 600 ng/band for Desidustat with 0.9979 regression coefficient. Standard spiking method showed method accuracy with a mean percentage recovery of 99.21%–101.63%. Limit of detection and limit of quantitation were found to be 3.94 and 11.94 ng/band, respectively. The method was found to be linear, precise, accurate, robust, rugged, selective, sensitive, and specific for the quantification of Desidustat in bulk and tablet dosage form and successfully can be applied for the qualitative and quantitative determination of Desidustat in bulk and marketed tablet formulation.","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2023-08-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"41993460","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}
{"title":"Miniaturized liquid extraction cartridge with a functional porous polytetrafluoroethylene membrane for the determination of formaldehyde in gaseous samples","authors":"","doi":"10.1002/sscp.202370076","DOIUrl":"https://doi.org/10.1002/sscp.202370076","url":null,"abstract":"","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2023-08-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47204398","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}
Ramya Thati, Seetha Bala Subrahanyam, A. Shaik, M. K. Mudiam
{"title":"Development, validation, and measurement uncertainty estimation of automated micro‐solid‐phase extraction coupled with liquid chromatography‐triple quadrupole mass spectrometry for the quantitative determination of anti‐tuberculosis drugs in milk samples","authors":"Ramya Thati, Seetha Bala Subrahanyam, A. Shaik, M. K. Mudiam","doi":"10.1002/sscp.202300088","DOIUrl":"https://doi.org/10.1002/sscp.202300088","url":null,"abstract":"","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2023-07-24","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"44826107","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}
{"title":"Development and validation of a reversed‐phase high‐performance liquid chromatography method for quantification of hesperidin from a nutraceutical","authors":"Vandana Panda, Swapnil Pund, Akash Saindane, Vidya Bokde","doi":"10.1002/sscp.202300053","DOIUrl":"https://doi.org/10.1002/sscp.202300053","url":null,"abstract":"","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2023-07-14","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"49170390","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}
N. Moustafa, Kout El‐Kloub Fars Mahmoud, Suilman A. Alderhami
{"title":"Overcoming shielding in mass detection via isolation of sulfur heterocycles using green silver nanoparticles","authors":"N. Moustafa, Kout El‐Kloub Fars Mahmoud, Suilman A. Alderhami","doi":"10.1002/sscp.202300034","DOIUrl":"https://doi.org/10.1002/sscp.202300034","url":null,"abstract":"","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2023-07-12","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"42200114","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}
{"title":"Chromatographic separation to determine doxycycline monohydrate and ornidazole","authors":"Bhoomi Patel, S. Patel","doi":"10.1002/sscp.202300061","DOIUrl":"https://doi.org/10.1002/sscp.202300061","url":null,"abstract":"","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2023-07-04","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47204648","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}
S. Chaudhary, K. C. Sharma, I. Sarangthem, A. Kar, P. Bhardwaj, Nanaocha Sharma, P. Mukherjee
{"title":"Reversed phase‐high‐performance liquid chromatography simultaneous estimation of phenolic compounds in hydroalcoholic extract of Potentilla fulgens root","authors":"S. Chaudhary, K. C. Sharma, I. Sarangthem, A. Kar, P. Bhardwaj, Nanaocha Sharma, P. Mukherjee","doi":"10.1002/sscp.202300048","DOIUrl":"https://doi.org/10.1002/sscp.202300048","url":null,"abstract":"","PeriodicalId":21639,"journal":{"name":"SEPARATION SCIENCE PLUS","volume":null,"pages":null},"PeriodicalIF":1.1,"publicationDate":"2023-07-02","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"47811822","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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