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Diclofenac Concentrations in Post-Mortem Specimens—Distribution, Case Reports, and Validated Method (UHPLC-QqQ-MS/MS) for Its Determination
The aim of the research was to establish a sensitive method for the quantification of diclofenac in postmortem samples. The developed method was applied in six cases: three fetuses in which the use of abortion pills by their mothers was suspected, one case of duodenal ulcer perforation, one case of...
Autores principales: | , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
MDPI
2022
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9332430/ https://www.ncbi.nlm.nih.gov/pubmed/35893854 http://dx.doi.org/10.3390/toxics10080421 |
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author | Szpot, Paweł Wachełko, Olga Zawadzki, Marcin |
author_facet | Szpot, Paweł Wachełko, Olga Zawadzki, Marcin |
author_sort | Szpot, Paweł |
collection | PubMed |
description | The aim of the research was to establish a sensitive method for the quantification of diclofenac in postmortem samples. The developed method was applied in six cases: three fetuses in which the use of abortion pills by their mothers was suspected, one case of duodenal ulcer perforation, one case of traffic accident with fatal outcome, and one acute renal failure in which the distribution of diclofenac was examined. The analyses were performed using liquid–liquid extraction of postmortem samples and the quantification of diclofenac via ultra-high performance liquid chromatography, coupled with triple quadrupole tandem mass spectrometry. Gradient elution using a C18 column was applied. Electrospray ionization measurement in positive multiple reaction monitoring mode was used. Diclofenac-d4 was used as an internal standard. The validation parameters were as follows: lower limit of quantification: 0.5 ng/mL, linearity of calibration curve: 0.5–500 ng/mL, intra- and interday accuracies and precisions: not greater than 15%; recovery values: 72.0–102.2%, and matrix effect: 2.2–28.0%. The developed method enabled the determination of diclofenac in human postmortem biological fluids (blood, urine, vitreous humor, bile, and stomach content), tissues (placenta, kidney, liver, and heart), and in exhumated fetus bones, with high recovery, sensitivity, precision, and accuracy. |
format | Online Article Text |
id | pubmed-9332430 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2022 |
publisher | MDPI |
record_format | MEDLINE/PubMed |
spelling | pubmed-93324302022-07-29 Diclofenac Concentrations in Post-Mortem Specimens—Distribution, Case Reports, and Validated Method (UHPLC-QqQ-MS/MS) for Its Determination Szpot, Paweł Wachełko, Olga Zawadzki, Marcin Toxics Article The aim of the research was to establish a sensitive method for the quantification of diclofenac in postmortem samples. The developed method was applied in six cases: three fetuses in which the use of abortion pills by their mothers was suspected, one case of duodenal ulcer perforation, one case of traffic accident with fatal outcome, and one acute renal failure in which the distribution of diclofenac was examined. The analyses were performed using liquid–liquid extraction of postmortem samples and the quantification of diclofenac via ultra-high performance liquid chromatography, coupled with triple quadrupole tandem mass spectrometry. Gradient elution using a C18 column was applied. Electrospray ionization measurement in positive multiple reaction monitoring mode was used. Diclofenac-d4 was used as an internal standard. The validation parameters were as follows: lower limit of quantification: 0.5 ng/mL, linearity of calibration curve: 0.5–500 ng/mL, intra- and interday accuracies and precisions: not greater than 15%; recovery values: 72.0–102.2%, and matrix effect: 2.2–28.0%. The developed method enabled the determination of diclofenac in human postmortem biological fluids (blood, urine, vitreous humor, bile, and stomach content), tissues (placenta, kidney, liver, and heart), and in exhumated fetus bones, with high recovery, sensitivity, precision, and accuracy. MDPI 2022-07-26 /pmc/articles/PMC9332430/ /pubmed/35893854 http://dx.doi.org/10.3390/toxics10080421 Text en © 2022 by the authors. https://creativecommons.org/licenses/by/4.0/Licensee MDPI, Basel, Switzerland. This article is an open access article distributed under the terms and conditions of the Creative Commons Attribution (CC BY) license (https://creativecommons.org/licenses/by/4.0/). |
spellingShingle | Article Szpot, Paweł Wachełko, Olga Zawadzki, Marcin Diclofenac Concentrations in Post-Mortem Specimens—Distribution, Case Reports, and Validated Method (UHPLC-QqQ-MS/MS) for Its Determination |
title | Diclofenac Concentrations in Post-Mortem Specimens—Distribution, Case Reports, and Validated Method (UHPLC-QqQ-MS/MS) for Its Determination |
title_full | Diclofenac Concentrations in Post-Mortem Specimens—Distribution, Case Reports, and Validated Method (UHPLC-QqQ-MS/MS) for Its Determination |
title_fullStr | Diclofenac Concentrations in Post-Mortem Specimens—Distribution, Case Reports, and Validated Method (UHPLC-QqQ-MS/MS) for Its Determination |
title_full_unstemmed | Diclofenac Concentrations in Post-Mortem Specimens—Distribution, Case Reports, and Validated Method (UHPLC-QqQ-MS/MS) for Its Determination |
title_short | Diclofenac Concentrations in Post-Mortem Specimens—Distribution, Case Reports, and Validated Method (UHPLC-QqQ-MS/MS) for Its Determination |
title_sort | diclofenac concentrations in post-mortem specimens—distribution, case reports, and validated method (uhplc-qqq-ms/ms) for its determination |
topic | Article |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9332430/ https://www.ncbi.nlm.nih.gov/pubmed/35893854 http://dx.doi.org/10.3390/toxics10080421 |
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