Rapid Determination of Non-Steroidal Anti-Inflammatory Drugs in Urine Samples after In-Matrix Derivatization and Fabric Phase Sorptive Extraction-Gas Chromatography-Mass Spectrometry Analysis
Fabric phase sorptive extraction (FPSE) has become a popular sorptive-based microextraction technique for the rapid analysis of a wide variety of analytes in complex matrices. The present study describes a simple and green analytical protocol based on in-matrix methyl chloroformate (MCF) derivatizat...
| Main Authors: | , , , |
|---|---|
| Format: | Article |
| Language: | English |
| Published: |
MDPI AG
2022-10-01
|
| Series: | Molecules |
| Subjects: | |
| Online Access: | https://www.mdpi.com/1420-3049/27/21/7188 |
| _version_ | 1797467125018787840 |
|---|---|
| author | Bharti Jain Rajeev Jain Abuzar Kabir Shweta Sharma |
| author_facet | Bharti Jain Rajeev Jain Abuzar Kabir Shweta Sharma |
| author_sort | Bharti Jain |
| collection | DOAJ |
| description | Fabric phase sorptive extraction (FPSE) has become a popular sorptive-based microextraction technique for the rapid analysis of a wide variety of analytes in complex matrices. The present study describes a simple and green analytical protocol based on in-matrix methyl chloroformate (MCF) derivatization of non-steroidal anti-inflammatory (NSAID) drugs in urine samples followed by FPSE and gas chromatography-mass spectrometry (GC-MS) analysis. Use of MCF as derivatizing reagent saves substantial amounts of time, reagent and energy, and can be directly performed in aqueous samples without any sample pre-treatment. The derivatized analytes were extracted using sol–gel Carbowax 20M coated FPSE membrane and eluted in 0.5 mL of MeOH for GC-MS analysis. A chemometric design of experiment-based approach was utilized comprising a Placket–Burman design (PBD) and central composite design (CCD) for screening and optimization of significant variables of derivatization and FPSE protocol, respectively. Under optimized conditions, the proposed FPSE-GC-MS method exhibited good linearity in the range of 0.1–10 µg mL<sup>−1</sup> with coefficients of determination (R<sup>2</sup>) in the range of 0.998–0.999. The intra-day and inter-day precisions for the proposed method were lower than <7% and <10%, respectively. The developed method has been successfully applied to the determination of NSAIDs in urine samples of patients under their medication. Finally, the green character of the proposed method was evaluated using ComplexGAPI tool. The proposed method will pave the way for simper analysis of polar drugs by FPSE-GC-MS. |
| first_indexed | 2024-03-09T18:49:13Z |
| format | Article |
| id | doaj.art-b20d7e0dfbf849a7bb87ea64b3887846 |
| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-09T18:49:13Z |
| publishDate | 2022-10-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-b20d7e0dfbf849a7bb87ea64b38878462023-11-24T06:00:10ZengMDPI AGMolecules1420-30492022-10-012721718810.3390/molecules27217188Rapid Determination of Non-Steroidal Anti-Inflammatory Drugs in Urine Samples after In-Matrix Derivatization and Fabric Phase Sorptive Extraction-Gas Chromatography-Mass Spectrometry AnalysisBharti Jain0Rajeev Jain1Abuzar Kabir2Shweta Sharma3Institute of Forensic Science & Criminology, Panjab University, Chandigarh 160014, IndiaCentral Forensic Science Laboratory, Forensic Toxicology Division, Plot #2, Sector 36-A, Dakshin Marg, Chandigarh 160036, IndiaDepartment of Chemistry and Biochemistry, Florida International University, Miami, FL 33199, USAInstitute of Forensic Science & Criminology, Panjab University, Chandigarh 160014, IndiaFabric phase sorptive extraction (FPSE) has become a popular sorptive-based microextraction technique for the rapid analysis of a wide variety of analytes in complex matrices. The present study describes a simple and green analytical protocol based on in-matrix methyl chloroformate (MCF) derivatization of non-steroidal anti-inflammatory (NSAID) drugs in urine samples followed by FPSE and gas chromatography-mass spectrometry (GC-MS) analysis. Use of MCF as derivatizing reagent saves substantial amounts of time, reagent and energy, and can be directly performed in aqueous samples without any sample pre-treatment. The derivatized analytes were extracted using sol–gel Carbowax 20M coated FPSE membrane and eluted in 0.5 mL of MeOH for GC-MS analysis. A chemometric design of experiment-based approach was utilized comprising a Placket–Burman design (PBD) and central composite design (CCD) for screening and optimization of significant variables of derivatization and FPSE protocol, respectively. Under optimized conditions, the proposed FPSE-GC-MS method exhibited good linearity in the range of 0.1–10 µg mL<sup>−1</sup> with coefficients of determination (R<sup>2</sup>) in the range of 0.998–0.999. The intra-day and inter-day precisions for the proposed method were lower than <7% and <10%, respectively. The developed method has been successfully applied to the determination of NSAIDs in urine samples of patients under their medication. Finally, the green character of the proposed method was evaluated using ComplexGAPI tool. The proposed method will pave the way for simper analysis of polar drugs by FPSE-GC-MS.https://www.mdpi.com/1420-3049/27/21/7188fabric phase sorptive extractiongas chromatography-mass spectrometrynon-steroidal anti-inflammatory drugsderivatizationurine analysis |
| spellingShingle | Bharti Jain Rajeev Jain Abuzar Kabir Shweta Sharma Rapid Determination of Non-Steroidal Anti-Inflammatory Drugs in Urine Samples after In-Matrix Derivatization and Fabric Phase Sorptive Extraction-Gas Chromatography-Mass Spectrometry Analysis Molecules fabric phase sorptive extraction gas chromatography-mass spectrometry non-steroidal anti-inflammatory drugs derivatization urine analysis |
| title | Rapid Determination of Non-Steroidal Anti-Inflammatory Drugs in Urine Samples after In-Matrix Derivatization and Fabric Phase Sorptive Extraction-Gas Chromatography-Mass Spectrometry Analysis |
| title_full | Rapid Determination of Non-Steroidal Anti-Inflammatory Drugs in Urine Samples after In-Matrix Derivatization and Fabric Phase Sorptive Extraction-Gas Chromatography-Mass Spectrometry Analysis |
| title_fullStr | Rapid Determination of Non-Steroidal Anti-Inflammatory Drugs in Urine Samples after In-Matrix Derivatization and Fabric Phase Sorptive Extraction-Gas Chromatography-Mass Spectrometry Analysis |
| title_full_unstemmed | Rapid Determination of Non-Steroidal Anti-Inflammatory Drugs in Urine Samples after In-Matrix Derivatization and Fabric Phase Sorptive Extraction-Gas Chromatography-Mass Spectrometry Analysis |
| title_short | Rapid Determination of Non-Steroidal Anti-Inflammatory Drugs in Urine Samples after In-Matrix Derivatization and Fabric Phase Sorptive Extraction-Gas Chromatography-Mass Spectrometry Analysis |
| title_sort | rapid determination of non steroidal anti inflammatory drugs in urine samples after in matrix derivatization and fabric phase sorptive extraction gas chromatography mass spectrometry analysis |
| topic | fabric phase sorptive extraction gas chromatography-mass spectrometry non-steroidal anti-inflammatory drugs derivatization urine analysis |
| url | https://www.mdpi.com/1420-3049/27/21/7188 |
| work_keys_str_mv | AT bhartijain rapiddeterminationofnonsteroidalantiinflammatorydrugsinurinesamplesafterinmatrixderivatizationandfabricphasesorptiveextractiongaschromatographymassspectrometryanalysis AT rajeevjain rapiddeterminationofnonsteroidalantiinflammatorydrugsinurinesamplesafterinmatrixderivatizationandfabricphasesorptiveextractiongaschromatographymassspectrometryanalysis AT abuzarkabir rapiddeterminationofnonsteroidalantiinflammatorydrugsinurinesamplesafterinmatrixderivatizationandfabricphasesorptiveextractiongaschromatographymassspectrometryanalysis AT shwetasharma rapiddeterminationofnonsteroidalantiinflammatorydrugsinurinesamplesafterinmatrixderivatizationandfabricphasesorptiveextractiongaschromatographymassspectrometryanalysis |