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Matrix solid-phase dispersion followed by liquid chromatography tandem 1 mass spectrometry for the determination of COXIBs in sewage sludge 2 samples 3
| Content Provider | Semantic Scholar |
|---|---|
| Author | Triñanes, Sara Casais, Carmen Mejuto, Carmen Cela, Rafael |
| Copyright Year | 2018 |
| Abstract | 9 A straightforward single-step extraction method based on matrix solid-phase 10 dispersion (MSPD), followed by high-performance liquid chromatography with 11 hybrid quadrupole time of flight mass spectrometry (LC-QTOF-MS), was 12 developed and optimized to determine five non-steroidal anti-inflammatory drugs 13 (Valdecoxib, Etoricoxib, Parecoxib, Celecoxib and 2,5-Dimethylcelecoxib) in 14 sewage sludge samples. The influence of different operational parameters on the 15 extraction efficiency a well as in the matrix effects of the produced extracts was 16 evaluated in detail. Under final working conditions, freeze dried samples (0.2 g) 17 were first soaked with 100 μL of aqueous potassium hydroxide solution (60%, 18 w/v), mixed with 1 g of anhydrous sodium sulfate and dispersed with 1 g of Florisil. 19 This blend was transferred to the top of a polypropylene column cartridge 20 containing 3 g of silica. Analytes were recovered using 15 mL of hexane/acetone 21 (1:2, v/v) mixture. The extracts were concentrated by evaporation and 22 reconstituted with 1mL of methanol/water (1:1, v/v), filtered and injected in the LC 23 system. Quantification limits from 0.005 and 0.05 ng g and absolute recoveries 24 ⃰ Author for correspondence, Phone: +34881814265, Fax:+34981547141 , e-mail: carmela.casais@usc.es (M.C.Casais) This is the accepted manuscript of the following article: Triñanes, S., Casais, M., Mejuto, M., & Cela, R. (2016). Matrix solid-phase dispersion followed by liquid chromatography tandem mass spectrometry for the determination of selective ciclooxygenase-2 inhibitors in sewage sludge samples. Journal Of Chromatography A, 1462, 35-43. doi: 10.1016/j.chroma.2016.07.044 © 2016 Elsevier B.V. This manuscript version is made available under the CC-BY-NC-ND 4.0 license (http:// creativecommons.org/licenses/by-nc-nd/4.0/) between 86 and 105% were achieved. Results indicated the presence of two of 25 the targeted COXIBs in real samples of sewage sludge, the highest average 26 concentration (22 ng g) corresponding to celecoxib. Moreover, the screening 27 capabilities of the LC-QTOF-MS system demonstrated that the developed MSPD 28 extraction procedure might be useful for the selective extraction of some other 29 pharmaceuticals (e.g. amiodarone and their metabolite N-desethylamiodarone, 30 miconazole, clotrimazole and ketoprofen) from sludge samples. 31 |
| File Format | PDF HTM / HTML |
| Alternate Webpage(s) | https://minerva.usc.es/xmlui/bitstream/handle/10347/17317/2016_journalchromatographyA_trinanes_matrix.pdf?isAllowed=y&sequence=17 |
| Language | English |
| Access Restriction | Open |
| Content Type | Text |
| Resource Type | Article |
