Vortex assisted liquid-liquid microextraction based on in situ formation of a natural deep eutectic solvent by microwave irradiation for the determination of beta-blockers in water samples.

In this study, a simple, green, and reliable method combining vortex-assisted liquid-liquid microextraction based on in situ formation of a novel hydrophobic natural deep eutectic solvent (NADES-VA-LLME) and high-performance liquid chromatography (HPLC) was developed for the determination of metoprolol and propranolol in water samples. The novel NADES was synthesized in situ within only 20 s by subjecting the water sample containing azelaic acid and thymol to microwave irradiation at 50 ˚C. Initial studies indicated that a 17:1 ratio of thymol to azelaic acid yielded the highest response for analytes. The influence of 7 parameters, including NADES volume, salt amount, sample pH, vortex time, centrifugation time, microwave time, and temperature, were screened using a 27-3 fractional factorial design. The obtained significant parameters were optimized by response surface methodology employing a Box-Behnken design. The method displayed satisfactory linearity (r=0.9996) for metoprolol and propranolol with limits of detection of 0.2 and 0.1 µg/L, respectively. The relative standard deviation at 2.5, 40, and 80 µg/L levels was lower than 6%, with accuracy in the range of 90.8-100.2%. Enrichment factors were 147.0 and 144.4 for metoprolol and propranolol, respectively. This study demonstrates that the developed in situ NADES-VA-LLME-HPLC technique can be considered as a fast and environmentally friendly alternative for isolation/preconcentration of ß-blockers from water samples.

Synthesis of hydroxy benzoin/benzil analogs and investigation of their antioxidant, antimicrobial, enzyme inhibition, and cytotoxic activities.

In this study, hydroxy benzoin ( 1-7 ), benzil ( 8-14 ), and benzoin/benzil-O-ß-D-glucosides ( 15-25 ) were synthesized to investigate their biological activities. An efficient method for synthesizing hydroxy benzoin compounds ( 1 - 7 ) was prepared from four different benzaldehydes using an ultrasonic bath. Then, antioxidant (FRAP, CUPRAC, and DPPH), antimicrobial (3 Gram (-), 4/6 Gram (+), one tuberculosis and one fungus), and enzyme inhibition (acetylcholinesterase, butyrylcholine esterase, tyrosinase, α-amylase, and α- glucosidase) for the all synthesized compounds ( 1-25 ) were evaluated. And also, four most active compounds ( 4 , 12 , 18a+b , and 25 ) from each group were evaluated to the human cervical cancer cell line (HeLa) and anticancer screening tests against the human retinal normal cell line (RPE). Compound 4 showed HeLa and RPE cancer cell activities as much as cisplatin. The synthesized compounds were characterized by spectroscopic methods (NMR, FT-IR, UV, LC-QTOF-MS) and the ACD NMR program's help.

Fast determination of anthocyanins and free pelargonidin in fruits, fruit juices, and fruit wines by high-performance liquid chromatography using a core-shell column.

Anthocyanins are water-soluble pigments that are liable for colors ranging from red to blue of most fruits, vegetables, and flowers. A novel and fast method was developed for the determination of five anthocyanins and free pelargonidin by high-performance liquid chromatography coupled to photodiode array detection. A 10% formic acid and acetonitrile mixture was employed as mobile phase in the gradient elution mode. Mobile phase composition, column temperature, flow rate, injection volume, and column conditioning time were optimized by employing a stepwise strategy. Using a C18 core-shell column (100 × 4.6 mm, 2.7 µm), the separation of six analytes was accomplished in less than 9.5 min with a run-to-run analysis time of 19 min. The developed method was validated with respect to linearity (r > 0.9999), limit of detection, limit of quantification, intra-/interday precision (<2%), accuracy (98.6-104.4%), and specificity. Afterwards, the method was applied to the determination of anthocyanins present in 15 different samples including fruits, fruit juices, and fruit wines.