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The use of conductive polymers (CPs) as a substrate in ambient paper spray ionization was achieved under high DC voltage.

publicado na web em 11/12/2017 This study shows that Fourier transform infrared (FTIR) spectroscopy, thermogravimetric analysis (TGA), and scanning electron microscopy (SEM) can be used as supporting tools for the evaluation of the quality of antiparasitics. In addition, an analytical methodology was developed and validated to quantify simultaneously thiabendazole (TB), febantel (FB), toltrazuril (TZ), and fluazuron (FZ) in bulk and in their veterinary pharmaceutical formulations using reverse phase high performance liquid chromatography (RP-HPLC). In order to investigate stability, pharmaceuticals were submitted to degradation processes under different conditions, such as recommended by the International Conference on Harmonization. The chromatographic conditions were optimized and the validation parameters, such as selectivity, linearity, detection limit, quantification limit, precision, accuracy, and robustness showed results within acceptable standards. All analytes were stable in the stability assays in acid and basic media and thermal conditions, except in the oxidation process, which presented two degradation peaks. Physicochemical characterization by TGA, FTIR, and SEM of raw materials of TB, FB, TZ, and FZ provided information about the authenticity of the analytes, proving the wide applicability of the instrumental techniques. The RP-HPLC proposed method was found to be accurate, precise, and reproducible and can in addition be used for routine quality control analysis.

This study aimed to show that the physicochemical proprieties obtained by Fourier transform infrared spectroscopy (FTIR), thermogravimetry (TG), and scanning electronic microscopy (SEM) can be useful tools for evaluating the quality of active pharmaceutical ingredients (APIs) and pharmaceutical products. In addition, a simple, sensitive, and efficient method employing HPLC-DAD was developed for simultaneous determination of lidocaine (LID), ciprofloxacin (CFX) and enrofloxacin (EFX) in raw materials and in veterinary pharmaceutical formulations. Compounds were separated using a Gemini C18 (250 mm × 4.6 mm, 5 µm) Phenomenex® column, at a temperature of 25 °C, with a mobile phase containing 10 mM of phosphoric acid (pH 3.29): acetonitrile (85.7:14.3, v/v) and a flow rate of 1.5 mL/min. Physicochemical characterization by TG, FTIR, and SEM of raw materials of LID, CFX, and EFX provided information useful for the evaluation, differentiation, and qualification of raw materials. Finally, the HPLC method was proved to be useful for evaluation of raw material and finished products, besides satisfying the need for an analytical method that allows simultaneous determination of EFX, CFX, and LID, which can also be extended to other matrices and applications.

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The assessment of selective molecularly imprinted solid-phase extraction (MISPE) for clean-up and extraction of cholesterol (CHO) from bovine and human serum samples was evaluated. Two molecular imprinted polymers (MIP) based on organic and inorganic/organic (hybrid) materials were obtained and compared regarding recovery and selectivity toward CHO. Optimum chromatographic separation between the CHO and its isobaric compound lathosterol (LATHO) has been achieved within 15 min using an Agilent Poroshell 120 EC-C18 column (120 mm × 3.0 mm, 2.7 μM) and mobile phase consisting of acetonitrile:methanol (8:2, v/v) at a flow rate of 0.6 mL min . Mass spectrometry detection was operated in atmospheric pressure chemical ionization (APCI) (+) mode and the SIM transitions [M - H O + H] for CHO and LATHO were 364.1 → 161.2 → 95.2 and 364.1 → 95.1 → 81.1 m/z, respectively. The sample preparation could be accomplished within 1 h, and the matrix effect on the MS signal after sample pretreatment did not interfere in the analyses. The method provided a good linear range (0.013-312 μM.) with coefficients of determination of R > 0.99, substantial sensitivity (limits of detection of 6.5 nM), good recovery (∼90%), high reproducibility (intraday and interday relative standard deviations less than 15%) and satisfactory accuracy (relative error ranged from -13.46% to 11.54%). The organic MIP showed superior performance compared with the hybrid. Finally, the MISPE procedure followed by LC-APCI-MS-MS analysis showed their suitable applicability to examine CHO and LATHO in serum samples.

An ultra-fast method for the simultaneous determination of heavy metals in Passiflora incarnata tea by capillary electrophoresis (CE) using a short-end injection combined with multivariate analysis was proposed. Separation was conducted by hydrodynamic injection (5 s at 0.5 psi) using the short-end injection procedure in a fused uncoated silica capillary (50 cm total length, 10.2 cm effective length, 50 µm i.d.) with separation time less than 2 min. An indirect UV detection at 214 nm was employed by using imidazole as a chromophore. The buffer used was 6 mmol/L hydroxybutyric acid (HIBA). The optimum conditions by full factorial with a central point were achieved by 18-crown-6 concentration (23.3 mmol L−1), voltage (+11.4 kV), methanol concentration (3.8%), and temperature (20 °C). The method showed good linearity (R2 > 0.998) for both Cd and Pb, inter-day precision of less than 14.49%, and an adequate limit of quantification only for Cd (LOQ < 0.5 µg mL−1 for Cd) based on the US Pharmacopeial Convention limit requirements for elemental impurities. After method validation, the method was applied to Passiflora incarnata tea samples from a local market. Furthermore, the developed method showed great potential for the determination of metals in other samples with proper sample preparation procedures.

Herein, an organic–inorganic hybrid molecularly imprinted polymer (MIP) was successfully synthesized with albendazole sulfoxide (ABZSO) as a template and 3-(trimethoxysilyl)propyl methacrylate, a bifunctional group compound, as a single cross-linking agent. In this study, a simple method using HPLC–DAD was developed for the determination of ABZSO enantiomers in human urine using pipette tip-based molecularly imprinted polymer solid phase extraction (PT–MIP–SPE). Enantioseparation with satisfactory retention times (5.17 and 7.09 min), acceptable theoretical plates (N = 4,535 and 5,091) and strong resolution (Rs = 5.45) was performed with an Agilent® Eclipse Plus C18 (100 mm × 4.6 mm, 3.5 μm) coupled with a Chiralpak® IA column (100 mm × 4.6 mm, 3 μm), a mixture with ethanol:water (50:50, v/v) as the mobile phase, temperature at 40°C, flow rate at 0.9 mL min−1 and λ = 230 nm. Thereafter, certain parameters affecting the PT–MIP–SPE were investigated in detail and the better conditions were: 300 μL of water as washing solvent, 500 μL of ethanol:acetic acid (9:1, v/v) as eluting solvent, 20 mg of MIP, 500 μL of human urine at pH 9 and no addition of NaCl. Recoveries/relative standard deviation (RSD%) for (R)-(+)-ABZSO and (S)-(−)-ABZSO were 78.2 ± 0.2% and 69.7 ± 1.7%, respectively.