To address sustainability issues, the green synthesis of nanomaterials has recently received considerable attention. This article addresses a novel and cost‐effective adsorbent for the extraction of eight phenyl‐N‐methylcarbamate insecticides from water samples. We first synthesized a magnetite/hydroxyapatite nanocomposite using snail shell powder via an environmental friendly approach. The morphology and physicochemical properties of magnetic hydroxyapatite were characterized by Fourier transform infrared spectroscopy, energy‐dispersive X‐ray spectroscopy, and scanning electron microscopy. Magnetic extraction parameters were optimized using a Doehlert matrix. Under optimum conditions, the magnetic extraction coupled with a LC–MS method shows good linearity with R2 ≥ 0.9982, suitable intra‐ and interday precision, and limits of detection and quantification in the range of 0.052–0.093 μg/L and 0.11–0.31 μg/L, respectively. Satisfactory relative recoveries of all carbamates were achieved from fortified water samples in the range of 93.89–101.01%.
A new ultra-high-performance liquid chromatography method for the simultaneous quantification of sofosbuvir, daclatasvir and ledipasvir was developed. Two combinations of these direct-acting antivirals are used in hepatitis C virus infection therapy and show high efficacy and safety. Fractional factorial design was used for screening the most influential factors on separation and time analysis. These significant factors were optimized using a central composite design. The optimum resolution was carried out by using a Waters XBridge C18 column (150 mm, 4.6 mm ID, 5 μm) at a temperature of 35°C ± 2°C and acetonitrile/sodium perchlorate buffer (10 mM, pH = 3.2) (40: 60 v/v) as mobile phase at a flow rate of 1.5 mL min−1. UV detection was set at λ = 210 nm. A short chromatographic separation time was achieved. The developed method was validated according to the accuracy profile approach and was found specific, precise, faithful and accurate. The detection limits were between 0.07 and 0.13 μg mL−1. Hence, this novel method can be employed for the routine quality control analysis and in dissolution profile studies of generics containing these products.
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