Thieli Schaefer Nunes, Lucas Schmidt, Kayla Peterson, Rosalind Wright, Julio Alberto Landero-Figueroa
{"title":"Iodine and Bromine Analysis in Human Urine and Serum by ICP-MS, Tailored for High-Throughput Routine Analysis in Population-Based Studies.","authors":"Thieli Schaefer Nunes, Lucas Schmidt, Kayla Peterson, Rosalind Wright, Julio Alberto Landero-Figueroa","doi":"10.3390/analytica7010006","DOIUrl":"10.3390/analytica7010006","url":null,"abstract":"<p><p>Iodine is essential for thyroid hormone synthesis and is particularly critical during pregnancy, where excess and mainly its deficiencies can impair fetal neurodevelopment and increase maternal complications. Bromine has also gained attention due to its potential to interfere with iodine metabolism and contribute to adverse health effects when present in excess. Monitoring iodine and bromine in biological samples, especially urine and serum, is therefore important for assessing thyroid function and population health. This work presents a simple and robust ICP-MS method for simultaneous determination of bromine and iodine in urine and serum. The procedure uses a 20-fold dilution with 10 mmol L<sup>-1</sup> ammonia containing 0.1% (<i>w</i>/<i>w</i>) EDTA-2Na, ensuring solution stability, minimizing sample-to-sample variability, and eliminating the need for matrix-matched calibration. EDTA-2Na effectively prevents precipitation of metal species at high pH, avoiding blockages in the sample introduction system. Method accuracy was confirmed through certified reference materials and spike-recovery experiments, both showing suitable agreement for the two analytes. Precision was consistently strong (RSD < 6%), and low detection limits were achieved (0.78 μg L<sup>-1</sup> for Br and 0.24 μg L<sup>-1</sup> for I). The use of a high-efficiency nebulizer enabled analysis with only 50 μL of sample, making the method suitable for limited-volume specimens. Overall, this approach provides a sensitive, accurate, and practical solution for large-scale population studies and clinical applications.</p>","PeriodicalId":521102,"journal":{"name":"Analytica (Basel, Switzerland)","volume":"7 1","pages":""},"PeriodicalIF":0.0,"publicationDate":"2026-03-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC13101949/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"147795953","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}
Annie Gathof, Tess Bonanno, Paige Rossicone, Adelaide E Clark
{"title":"Improved and Novel Methods for Investigating Organophosphate Esters in Particulate Matter.","authors":"Annie Gathof, Tess Bonanno, Paige Rossicone, Adelaide E Clark","doi":"10.3390/analytica5040032","DOIUrl":"10.3390/analytica5040032","url":null,"abstract":"<p><p>A pressurized liquid extraction (PLE) method for the extraction of 31 organophosphate esters (OPEs) and novel organophosphate esters (NOPEs) has been developed. Unlike previously published methods, this method utilizes the high-throughput nature of PLE (as opposed to Soxhlet or sonication methods) without using potentially harmful organic solvents like methylene chloride. Combinations of hexane and acetone and hexane and ethyl acetate at various temperatures were examined. Extracts were concentrated and analyzed via gas chromatography-mass spectrometry. The final optimized method utilized 1:1 <i>v</i>/<i>v</i> hexane/ethyl acetate at 100 °C for three static cycles (5 min each) at 80% flush volume and a 100 s N<sub>2</sub> purge. This provided average surrogate corrected target analyte percent recoveries in spike and recovery experiments (<i>n</i> = 6) for OPEs and NOPEs of 106 ± 13%, with average surrogate recoveries of 88.6 ± 7.3%. The developed method was further validated using standard reference materials and was then applied to atmospheric particulate matter samples collected in the city of Providence, RI. The dataset reflected ambient concentrations of 16 OPEs and NOPEs (reported in pg m<sup>-3</sup>) for the first time in the greater Providence metropolitan area, including one of the first reports of NOPEs in atmospheric particulate matter in the U.S.</p>","PeriodicalId":521102,"journal":{"name":"Analytica (Basel, Switzerland)","volume":"5 4","pages":"471-480"},"PeriodicalIF":0.0,"publicationDate":"2024-12-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"https://www.ncbi.nlm.nih.gov/pmc/articles/PMC12621544/pdf/","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"145553087","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"OA","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}