| Article ID | Journal | Published Year | Pages | File Type |
|---|---|---|---|---|
| 1220774 | Journal of Pharmaceutical and Biomedical Analysis | 2015 | 9 Pages |
•A simple and efficient method was developed for determination of NSAIDs.•It was compared with a LDS-DLLME method to demonstrate its capabilities.•It has more pre-concentrating ability than other methods using equal sample volume.•Gas chromatography-flame ionization detector was used, with no derivatization step.•The method has been satisfactorily applied to the analysis of human urine samples.
Two dispersive-based liquid–liquid microextraction methods including ultrasound-enhanced air-assisted liquid–liquid microextraction (USE-AALLME) and low-density solvent-based dispersive liquid–liquid microextraction (LDS-DLLME) were compared for the extraction of salicylic acid (the hydrolysis product of acetylsalicylic acid), diclofenac and ibuprofen, as instances of the most commonly used nonsteroidal anti-inflammatory drugs (NSAIDs), in human urine prior to their determination by gas chromatography with flame ionization detection (GC-FID). The influence of different parameters affecting the USE-AALLME (including type and volume of the extraction solvent, sample pH, ionic strength, and simultaneous sonication and number of extraction cycles) and the LDS-DLLME (including type and volume of the extraction and disperser solvents, sample pH, and ionic strength) were investigated to optimize their extraction efficiencies. Both methods are fast, simple and convenient with organic solvent consumption at μL level. However, the best results were obtained using the USE-AALLME method, applying 30 μL of 1-octanol as extraction solvent, 5.0 mL of sample at pH 3.0, without salt addition, and 5 extraction cycles during 20 s of sonication. This method was validated based on linearities (r2 > 0.971), limits of detection (0.1–1.0 μg L−1), linear dynamic ranges (0.4–1000.0 μg L−1), enrichment factors (115 ± 3–135 ± 3), consumptive indices (0.043–0.037), inter- and intra-day precisions (4.3–4.8 and 5.6–6.1, respectively), and relative recoveries (94–103%). The USE-AALLME in combination with GC-FID, and with no need to derivatization step, was demonstrated to be a simple, inexpensive, sensitive and efficient method to determine NSAIDs in human urine samples.
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