LCGC EuropePub Date : 2022-10-01DOI: 10.56530/lcgc.eu.dk3677x5
R. Mcdowall
{"title":"What Are Orphan Data?","authors":"R. Mcdowall","doi":"10.56530/lcgc.eu.dk3677x5","DOIUrl":"https://doi.org/10.56530/lcgc.eu.dk3677x5","url":null,"abstract":"The term orphan data is used frequently in the context of data integrity. What does it mean for chromatography data systems? How can we prevent or detect orphan data?","PeriodicalId":402085,"journal":{"name":"LCGC Europe","volume":"23 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2022-10-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"123480827","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}
LCGC EuropePub Date : 2022-09-01DOI: 10.56530/lcgc.eu.od3570x2
Jinxiang Li, Jun Liu, Qianfeng Weng
{"title":"A Hydrophilic Strong Anion-Exchange Hybrid Monolith for Capillary Liquid Chromatography","authors":"Jinxiang Li, Jun Liu, Qianfeng Weng","doi":"10.56530/lcgc.eu.od3570x2","DOIUrl":"https://doi.org/10.56530/lcgc.eu.od3570x2","url":null,"abstract":"A hydrophilic strong anion-exchange monolithic hybrid column was prepared by in-capillary coating 5-µm bare silica particles with the copolymers of methacryloxyethyltrimethyl ammonium chloride and pentaerythritol triacrylate in the presence of a porogen consisting of water, methanol, and cyclohexanol. The composition of the porogen and the concentration of the monomers were investigated and selected. The resulting column was characterized. The column had an uniform pore structure and could withstand a back pressure up to 3500 psi. Its permeability was comparable to that of packed columns and the swelling-shrinking behaviour negligible. Its hydrophobicity could be suppressed at acetonitrile concentrations above 40% (v/v) and the minimum theoretical plate height was about 10 µm for BrÑ. The column-to-column relative standard deviations (RSDs) were 2.2% and 3.5% (n = 9) and the batch-to-batch RSDs were 2.4% and 5.5% (n = 3) for k and H values, respectively. The column exhibited a remarkable performanceforthe separation of inorganic anions, organic weak acids, phenols, and nucleotides.","PeriodicalId":402085,"journal":{"name":"LCGC Europe","volume":"1 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2022-09-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"130375077","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}
LCGC EuropePub Date : 2022-07-01DOI: 10.56530/lcgc.eu.qd8477p7
Jakub Tomasko, David Maxa, K. Navratilova, Tomas Kourimsky, V. Hrbek, J. Hajšlová, J. Pulkrabová
{"title":"Application of Liquid- and Supercritical Fluid Chromatography Coupled with High-Resolution Mass Spectrometry for the Analysis of Short-, Medium-, and Long-Chain Chlorinated Paraffins in Dietary Supplements","authors":"Jakub Tomasko, David Maxa, K. Navratilova, Tomas Kourimsky, V. Hrbek, J. Hajšlová, J. Pulkrabová","doi":"10.56530/lcgc.eu.qd8477p7","DOIUrl":"https://doi.org/10.56530/lcgc.eu.qd8477p7","url":null,"abstract":"Chlorinated paraffins (CPs) are an emerging and ubiquitous group of environmental pollutants associated with adverse effects on human health, including endocrine disruption and possible carcinogenicity. In this study, supercritical fluid chromatography (SFC) and ultrahigh-performance liquid chromatography (UHPLC) — both coupled with high-resolution mass spectrometry (HRMS) — methods for the analysis of short-, medium-, and long-chain CPs in fish oil-based dietary supplements were developed and validated at concentration levels of 0.6 and 3.0 µg/g lipid weight (lw). The recoveries were in the range of 80–96% and repeatabilities, expressed as relative standard deviations, were <19%. The limits of detection for the UHPLC–HRMS method (from 0.03 to 0.05 µg/g lw) were 5 to 10 times lower than those obtained by SFC–HRMS (from 0.13 to 0.50 µg/lw).","PeriodicalId":402085,"journal":{"name":"LCGC Europe","volume":"49 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2022-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"121560656","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}
LCGC EuropePub Date : 2022-07-01DOI: 10.56530/lcgc.eu.ue1079n4
Chris Burgess
{"title":"Quo Vadis Analytical Procedure Development and Validation?","authors":"Chris Burgess","doi":"10.56530/lcgc.eu.ue1079n4","DOIUrl":"https://doi.org/10.56530/lcgc.eu.ue1079n4","url":null,"abstract":"What do the draft publications ICH Q2(R2) and Q14 for analytical procedure validation and development mean for a regulated good manufacturing practice (GMP) laboratory? Are they consistent with the approach taken by the United States Pharmacopeia (USP) <1220> on Analytical Procedure Life Cycle? Why does it take the ICH two documents to describe what the USP can do in one?","PeriodicalId":402085,"journal":{"name":"LCGC Europe","volume":"86 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2022-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"131500710","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}
LCGC EuropePub Date : 2022-07-01DOI: 10.56530/lcgc.eu.tp4376p2
Marise van der Vegt, Ruben Kause, B. Berendsen, Stefan van Leeuwen
{"title":"Dispersive Solid-Phase Extraction and Solid-Phase Extraction for ppt-level PFAS Analysis in Apples: A Comparison","authors":"Marise van der Vegt, Ruben Kause, B. Berendsen, Stefan van Leeuwen","doi":"10.56530/lcgc.eu.tp4376p2","DOIUrl":"https://doi.org/10.56530/lcgc.eu.tp4376p2","url":null,"abstract":"Per- and polyfluoralkyl substances (PFAS) are found in our food. Sensitive, precise, and accurate analytical methods are needed to estimate human exposure to these chemicals. A comparative study was performed between two extraction and cleanup methods (solid-phase extraction [SPE] and dispersive SPE) for the analysis of PFAS in apples. Both methods showed excellent sensitivity, precision, and accuracy. dSPE has some benefits over conventional SPE, and vice versa. The advantages and disadvantages of both methods are discussed.","PeriodicalId":402085,"journal":{"name":"LCGC Europe","volume":"21 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2022-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"125661573","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}
LCGC EuropePub Date : 2022-07-01DOI: 10.56530/lcgc.eu.uf5786p6
I. H. Ahmad, G. L. Losacco, E. Regalado
{"title":"Nonlinear Predictive Modelling Enables In Silico Optimization of Chromatographic Methods for Complex Stationary Phase‑Analyte Interactions","authors":"I. H. Ahmad, G. L. Losacco, E. Regalado","doi":"10.56530/lcgc.eu.uf5786p6","DOIUrl":"https://doi.org/10.56530/lcgc.eu.uf5786p6","url":null,"abstract":"The development of robust analytical assays for separation and analysis of complex multicomponent mixtures can often be challenging, reflecting the increased complexity of new medicine and vaccine processes. In silico liquid chromatography (LC) method development strategies for small molecules have reached a mature stage across the pharmaceutical industry. However, a straightforward approach for large molecules remains elusive because of conformational changes that can often influence chromatographic retention. Nonetheless, an excellent correlation between experimental and predicted retention time is possible by deploying the correct regression retention models in terms of ln k vs. %B and ln k vs. 1/T (ΔtR < 0.1%). Excellent outcomes generated through in silico chromatographic method development of large molecules using different chaotropic and denaturing mobile phases are illustrated. Linear and nonlinear (polynomial regression) retention models using readily available software were deployed as a function of several chromatographic parameters (gradient slope and column temperature) for a variety of proteins (12–670 kDa) and peptides.","PeriodicalId":402085,"journal":{"name":"LCGC Europe","volume":"8 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2022-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"116915915","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}
LCGC EuropePub Date : 2022-07-01DOI: 10.56530/lcgc.eu.bl7965l5
Tomas Kourimsky, V. Hrbek, Martin Steidl, J. Hajšlová
{"title":"Analysis of MCPD and Glycidyl Fatty Acid Esters in Refined Plant Oils by Supercritical Fluid Chromatography– High-Resolution Mass Spectrometry","authors":"Tomas Kourimsky, V. Hrbek, Martin Steidl, J. Hajšlová","doi":"10.56530/lcgc.eu.bl7965l5","DOIUrl":"https://doi.org/10.56530/lcgc.eu.bl7965l5","url":null,"abstract":"2- and 3-chloropropane-1,2-diol (2- and 3-MCPD) and their fatty acid esters (2- and 3-MCPDEs) together with glycidyl fatty acids esters (GEs) belong to a group of process-induced contaminants. They are formed in high temperature environments and most commonly occur in refined vegetable oils. Since 2021, maximum limits for GEs and 3-MCPDEs have been enforceable in the EU, and the requirement for adequate analytical methods is constantly increasing. The aim of this study was to develop an efficient method to enable a rapid determination of nine 3-MCPDEs and seven GEs in vegetable oils within a single run employing supercritical fluid chromatography coupled to high-resolution tandem mass spectrometry (SFC–HRMS/MS). Contrary to a routine gas chromatography mass spectrometry method aimed at determination of the total MCPD pool, the sample throughput when using SFC–HRMS/MS was greatly increased, as the “dilute-and shoot” approach did not require any hydrolysis and derivatization. Additionally, the pattern of natural MCPDEs was characterized. The performance characteristics of this new method met the criteria required by Commision Regulation 2019/2093 for all target analytes.","PeriodicalId":402085,"journal":{"name":"LCGC Europe","volume":"14 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2022-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"127960686","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}
LCGC EuropePub Date : 2022-07-01DOI: 10.56530/lcgc.eu.ig4675a1
Jana Kvirencova, V. Hrbek, M. Tomaniová, J. Hajšlová
{"title":"Authentication of Panax Ginseng‑Based Herbal Teas Using “Chemical Markers” Strategy","authors":"Jana Kvirencova, V. Hrbek, M. Tomaniová, J. Hajšlová","doi":"10.56530/lcgc.eu.ig4675a1","DOIUrl":"https://doi.org/10.56530/lcgc.eu.ig4675a1","url":null,"abstract":"This article describes the method development involved in the authentication of nutraceuticals, particularly those containing Panax ginseng, which is popular because of possible positive effects on human health. For this purpose, an analytical strategy based on a metabolomic approach was chosen. The aqueous methanolic extracts were analyzed using ultrahigh-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC–HRMS). Generated data were processed by advanced statistical methods that enabled the specific markers for Panax ginseng and other plants that can be used for its adulteration (Gynostemma pentaphyllum, Withania somnifera, Eleutherococcus senticosus) to be found. The developed method is primarily intended for verifying the presence of Panax ginseng and its adulterants in Panax ginseng-based herbal teas.","PeriodicalId":402085,"journal":{"name":"LCGC Europe","volume":"42 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2022-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"132751852","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}
LCGC EuropePub Date : 2022-07-01DOI: 10.56530/lcgc.eu.wi6189z4
L. Drábová, Lenka Libenská, Markéta Zedníková, Veronika Vondrášková, J. Hajšlová, J. Pulkrabová
{"title":"Analysis of UV-Treated Mushrooms: Dietary Source of Vitamin D2?","authors":"L. Drábová, Lenka Libenská, Markéta Zedníková, Veronika Vondrášková, J. Hajšlová, J. Pulkrabová","doi":"10.56530/lcgc.eu.wi6189z4","DOIUrl":"https://doi.org/10.56530/lcgc.eu.wi6189z4","url":null,"abstract":"In recent years, dietary intake of vitamin D has become an issue of high concern because this bioactive molecule boosts the immune system and is presumed to provide some protection against Covid-19. Under these conditions, a search for nontraditional dietary sources has appeared as a new challenge. One of the possibilities is irradiation of champignons that contain a high amount of ergosterol, a vitamin D2 precursor. In our study, a fast and sensitive liquid chromatography coupled to tandem mass spectrometry (LC–MS/MS) method for the determination of vitamin D2 in fresh mushrooms and its metabolite 25(OH)D2 in the blood of volunteers regularly consuming UV-treated mushrooms has been introduced. For extraction of desiccated mushrooms, solid-liquid extraction n-hexane–ethyl acetate was used, and n-hexane was employed for blood plasma samples. Separation of target analytes was performed on a polymeric bonding C18 phase column. Satisfactory limits of quantification (LOQs) were reached both for the control of vitamin D2 content in mushrooms (LOQ = 10 ng/g) and for the monitoring of vitamin D2 and D3 metabolite in human blood (LOQ = 2.5 ng/mL). For accurate quantification, isotopic dilution was employed.","PeriodicalId":402085,"journal":{"name":"LCGC Europe","volume":"66 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2022-07-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"124210250","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}
LCGC EuropePub Date : 2022-06-01DOI: 10.56530/lcgc.eu.jk3969w4
Kris Morreel, R. T'kindt, G. Debyser, Stefanie Jonckheere, P. Sandra
{"title":"Diving into the Structural Details of In Vitro Transcribed mRNA Using Liquid Chromatography–Mass Spectrometry-Based Oligonucleotide Profiling","authors":"Kris Morreel, R. T'kindt, G. Debyser, Stefanie Jonckheere, P. Sandra","doi":"10.56530/lcgc.eu.jk3969w4","DOIUrl":"https://doi.org/10.56530/lcgc.eu.jk3969w4","url":null,"abstract":"The production process of in vitro transcribed messenger RNA (IVT-mRNA)-based vaccines has matured in recent years, partly due to the fight against infectious diseases such as COVID-19. One key to success has been the use of modified, next to canonical, nucleotides and the efficient addition of a Cap-structure and poly A tail to the 5’ and 3’ end, respectively, of this massive biomolecule. These important features affect mRNA stability and impact translation efficiency, consequently boosting the optimization and implementation of liquid chromatography–mass spectrometry (LC–MS)-based oligonucleotide profiling methods for their characterization. This article will provide an overview of these LC–MS methods at a fundamental and application level. It will be shown how LC–MS is implemented in mRNA-based vaccine analysis to determine the capping efficiency and the poly A tail length, and how it allows, via RNA mapping, (i) to determine the mRNA sequence, (ii) to screen the fidelity of the manufactured modifications, and (iii) to identify and quantify unwanted modifications resulting from manufacturing or storage, and sequence variants resulting from mutation or transcription errors.","PeriodicalId":402085,"journal":{"name":"LCGC Europe","volume":"44 1","pages":"0"},"PeriodicalIF":0.0,"publicationDate":"2022-06-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"124795610","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}