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...
| Main Authors: | , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
MDPI AG
2022-07-01
|
| Series: | Toxics |
| Subjects: | |
| Online Access: | https://www.mdpi.com/2305-6304/10/8/421 |
| _version_ | 1797407705006080000 |
|---|---|
| author | Paweł Szpot Olga Wachełko Marcin Zawadzki |
| author_facet | Paweł Szpot Olga Wachełko Marcin Zawadzki |
| author_sort | Paweł Szpot |
| collection | DOAJ |
| 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. |
| first_indexed | 2024-03-09T03:45:23Z |
| format | Article |
| id | doaj.art-6a68d48d8e9d4ba792fabf24a8e64542 |
| institution | Directory Open Access Journal |
| issn | 2305-6304 |
| language | English |
| last_indexed | 2024-03-09T03:45:23Z |
| publishDate | 2022-07-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Toxics |
| spelling | doaj.art-6a68d48d8e9d4ba792fabf24a8e645422023-12-03T14:34:36ZengMDPI AGToxics2305-63042022-07-0110842110.3390/toxics10080421Diclofenac Concentrations in Post-Mortem Specimens—Distribution, Case Reports, and Validated Method (UHPLC-QqQ-MS/MS) for Its DeterminationPaweł Szpot0Olga Wachełko1Marcin Zawadzki2Department of Forensic Medicine, Wroclaw Medical University, 50345 Wroclaw, PolandInstitute of Toxicology Research, 45 Kasztanowa Street, 55093 Borowa, PolandDepartment of Forensic Medicine, Wroclaw Medical University, 50345 Wroclaw, PolandThe 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.https://www.mdpi.com/2305-6304/10/8/421diclofenacUHPLC-QqQ-MS/MSabortiondistributionfetus |
| spellingShingle | Paweł Szpot Olga Wachełko Marcin Zawadzki Diclofenac Concentrations in Post-Mortem Specimens—Distribution, Case Reports, and Validated Method (UHPLC-QqQ-MS/MS) for Its Determination Toxics diclofenac UHPLC-QqQ-MS/MS abortion distribution fetus |
| 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 | diclofenac UHPLC-QqQ-MS/MS abortion distribution fetus |
| url | https://www.mdpi.com/2305-6304/10/8/421 |
| work_keys_str_mv | AT pawełszpot diclofenacconcentrationsinpostmortemspecimensdistributioncasereportsandvalidatedmethoduhplcqqqmsmsforitsdetermination AT olgawachełko diclofenacconcentrationsinpostmortemspecimensdistributioncasereportsandvalidatedmethoduhplcqqqmsmsforitsdetermination AT marcinzawadzki diclofenacconcentrationsinpostmortemspecimensdistributioncasereportsandvalidatedmethoduhplcqqqmsmsforitsdetermination |