Ibuprofen, Carbamazepine and β-Estradiol Determination Using Thin-Film Microextraction and Gas Chromatography-Mass Spectrometry

Abstract

The use of thin-film microextraction for the extraction of selected pharmaceutical compounds followed by gas chromatography-mass spectrometry detection was evaluated. A segment of polysiloxanes polymer sheet was used as low cost, single use, disposable extraction phase, while Milli-Q water spiked at 20 µg L −1 with the analytes was used for the optimization assays. The controlling parameters for the extraction were optimized via experimental design and it was found that an extraction time of 3 h using a sample volume of 1000 mL at pH 4 with the addition of 20% methanol and 20% sodium chloride provided the greatest extraction efficiency. Recoveries between 67.1 and 85.0% were achieved, with a repeteability lower than 20% (expressed as coefficient of variation) and limit of detection ranged from 0.41 and 0.92 µg L −1 . The proposed method show similar analytical performance when compared to the determination of the analytes using stir bar sorptive extraction.

Carbon-Based Sorbent Coatings for the Determination of Pharmaceutical Compounds by Bar Adsorptive Microextraction

“…As it can be observed, the developed methodology using BAμE devices coated with sucrose-based hydrochar presents similar or better recovery yields than other miniaturized enrichment techniques, e.g., SBSE coated with PDMS, PA or EG [38] or SBME coated with C8 polymer [39] for the extraction of carbamazepine; TFME coated with PDMS [44] for the extraction of 17--estradiol; SBSE coated with PDMS [42] for the extraction of clofibric acid; SBSE coated with PU [45] for the extraction of diclofenac, gemfibrozil or mefenamic acid. Additionally, the BAμE(npHS)-μLD/HPLC-DAD methodology sensitivity is similar when compared to analogue instrumental systems [37,39,45] and/or some mass spectrometry or tandem mass 26/40 spectrometry instrumental systems [40,44]. On the other hand, instrumental apparatus that employ mass spectrometry or tandem mass spectrometry expectedly presented lower LODs than the proposed technique [38,41,44,46].…”

“…Additionally, the BAμE(npHS)-μLD/HPLC-DAD methodology sensitivity is similar when compared to analogue instrumental systems [37,39,45] and/or some mass spectrometry or tandem mass 26/40 spectrometry instrumental systems [40,44]. On the other hand, instrumental apparatus that employ mass spectrometry or tandem mass spectrometry expectedly presented lower LODs than the proposed technique [38,41,44,46].…”

“…Compared with the commercially available and widespread used SBSE­(PDMS) device, the system BAμE­(HS/LiZn180)/HPLC-DAD allows 82 and 72% recovery at LOD of 2.0 μg L –1 of two hormones 17-α-ethinylestradiol and estrone, respectively, while the commercial device presents recoveries between 9 and 50% even using MS detectors. Additionally, the BAμE­(HS/LiZn180)-μLD/HPLC-DAD methodology sensitivity to all analytes is similar when compared to analogue instrumental systems, or even with some mass spectrometry or tandem mass spectrometry instrumental systems in the case of carbamazepine, sulfamethoxazole, 17-β-estradiol, 17-α-ethinyl­estradiol, and estrone. − …”

“…A comparison of the performance of the BAμE(npHS)-μLD/HPLC-DAD methodology and other established static-based microextraction techniques is shown in table 3 [36][37][38][39][40][41][42][43][44]. As it can be observed, the developed methodology using BAμE devices coated with sucrose-based hydrochar presents similar or better recovery yields than other miniaturized enrichment techniques, e.g., SBSE coated with PDMS, PA or EG [38] or SBME coated with C8 polymer [39] for the extraction of carbamazepine; TFME coated with PDMS [44] for the extraction of 17--estradiol; SBSE coated with PDMS [42] for the extraction of clofibric acid; SBSE coated with PU [45] for the extraction of diclofenac, gemfibrozil or mefenamic acid. Additionally, the BAμE(npHS)-μLD/HPLC-DAD methodology sensitivity is similar when compared to analogue instrumental systems [37,39,45] and/or some mass spectrometry or tandem mass 26/40 spectrometry instrumental systems [40,44].…”

“…38,40−48 As can be observed, the developed methodology using BAμE devices coated with low-T activated hydrochar HS/LiZn180 presents similar or better recovery yields than other miniaturized enrichment techniques most of times in similar pH conditions. For example, SBSE coated with PDMS, PA or EG, 42 or SBME coated with C8 polymer 43 for the extraction of carbamazepine; TFME coated with PDMS 46 for the extraction of 17-β-estradiol; SBSE coated with PDMS 48 for the extraction of clofibric acid; SBSE coated with PU 47 for the extraction of diclofenac, gemfibrozil, or mefenamic acid. Compared with the commercially available and widespread used SBSE(PDMS) device, the system BAμE(HS/LiZn180)/ HPLC-DAD allows 82 and 72% recovery at LOD of 2.0 μg L −1 of two hormones 17-α-ethinylestradiol and estrone, respectively, while the commercial device presents recoveries between 9 and 50% even using MS detectors.…”