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Determination of Non-Steroidal Anti-Inflammatory Drugs in Animal Urine Samples by Ultrasound Vortex-Assisted Dispersive Liquid–Liquid Microextraction and Gas Chromatography Coupled to Ion Trap-Mass Spectrometry
| Content Provider | MDPI |
|---|---|
| Author | Avino, Pasquale Notardonato, Ivan Passarella, Sergio Russo, Mario Vincenzo |
| Copyright Year | 2020 |
| Description | A low solvent consumption method for the determination of non-steroidal anti-inflammatory drugs (NSAIDs) in animal urine samples is studied. The NSAIDs were extracted with CH2Cl2 by the ultrasound vortex assisted dispersive liquid–liquid microextraction (USVA-DLLME) method from urine samples, previously treated with β-glucuronidase/acrylsulfatase. After centrifugation, the bottom phase of the chlorinated solvent was separated from the liquid matrix, dried with Na2SO4, and derivatized with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) + trimethylchlorosilane (TMCS) (99 + 1). After cooling at room temperature, the solution was concentrated under nitrogen flow, and 1 µL of solution was analyzed in gas chromatography/ion trap-mass spectrometry (GC-IT-MS). The enrichment factor was about 300–450 times and recoveries ranged from 94.1 to 101.2% with a relative standard deviation (RSD) of ≤4.1%. The USVA-DLLME process efficiency was not influenced by the characteristics of the real urine matrix; therefore, the analytical method characteristics were evaluated in the range 1–100 ng mL−1 (R2 ≥ 0.9950). The limits of detection (LODs) and limits of quantification (LOQs) were between 0.1 and 0.2 ng mL−1 with RSD ≤4.5% and between 4.1 and 4.7 ng mL−1 with RSD ≤3.5%, respectively, whereas inter- and intra-day precision was 3.8% and 4.5%, respectively. The proposed analytical method is reproducible, sensitive, and simple. |
| Starting Page | 5441 |
| e-ISSN | 20763417 |
| DOI | 10.3390/app10165441 |
| Journal | Applied Sciences |
| Issue Number | 16 |
| Volume Number | 10 |
| Language | English |
| Publisher | MDPI |
| Publisher Date | 2020-08-06 |
| Access Restriction | Open |
| Subject Keyword | Applied Sciences Analytical Chemistry Non-steroidal Anti-inflammatory Drug (nsaid) Urine Doping Analysis Dispersive Liquid–liquid Microextraction (dllme) Gas Chromatography Mass Spectrometry (gc-ms) |
| Content Type | Text |
| Resource Type | Article |
