Characterization of the antibiotic doripenem using physicochemical methods: chromatography, spectrophotometry, spectroscopy and thermal analysis

Doripenem was characterized through physicochemical and spectroscopic techniques, as well as thermal analysis. TLC (Rf = 0.62) and HPLC (rt = 7.4 min) were found to be adequate to identify the drug. UV and infrared spectra showed similar profile between doripenem bulk and standard. The ¹H and 13C NMR analysis revealed chemical shifts that allowed identifying the drug. Thermal analysis demonstrated three steps with mass loss, at 128, 178 and 276 ºC. The work was successfully applied to qualitative analysis of doripenem, showing the reported methods can be used for physicochemical characterization of doripenem

Estudio de la contaminación por metales en sedimentos acuáticos de la Bahía de Matanzas

Surface sediments of the Bay of Matanzas (Cuba) were studied to assess its environmental quality by using several criteria (metal content index, pollution load index and sediment quality guidelines). Two partial digestion sediment procedures and a modified BCR sequential extraction were used. The concentrations of metals were measured by atomic spectroscopy methods. The founded contents of Cu (2,4-27,9 mg kg-1), Zn (2,5-55,5 mg kg-1) and Ni (8,8-99,2 mg kg-1) were below those reported by other authors. The results obtained suggested that the most polluted sites were 3, 5, and 6. The sequential extraction procedure showed that most of the studied metals were associated to the more stable fractions.

Authenticity study of Phyllanthus species by NMR and FT-IR Techniques coupled with chemometric methods

The importance of medicinal plants and their use in industrial applications is increasing worldwide, especially in Brazil. Phyllanthus species, popularly known as "quebra-pedras" in Brazil, are used in folk medicine for treating urinary infections and renal calculus. This paper reports an authenticity study, based on herbal drugs from Phyllanthus species, involving commercial and authentic samples using spectroscopic techniques: FT-IR, ¹H HR-MAS NMR and ¹H NMR in solution, combined with chemometric analysis. The spectroscopic techniques evaluated, coupled with chemometric methods, have great potential in the investigation of complex matrices. Furthermore, several metabolites were identified by the NMR techniques.

Stability-indicating comparative methods using mekc and lc for determination of olmesartan medoxomil

A stability-indicating method using MEKC was validated for the analysis of olmesartan medoxomil in tablets. Successful separation was achieved using a fused silica capillary (40 cm x 50 µm i.d.); background electrolyte consisted of a combination of 10 mmol L-1 borate buffer and 5 mmol L-1 anionic detergent sodium dodecyl sulfate (95:5; v/v) pH 6.5; hydrodynamic mode at 50 mBar for 5 s; 25 kV separation voltage at 25 ºC; and column temperature 25 ºC with detection at 257 nm. The proposed method, validated following ICH guidelines, was applied to the determination of this antihypertensive with good results compared with an LC method.

Cat's claw oxindole alkaloid isomerization induced by common extraction methods

Cat's claw oxindole alkaloids are prone to isomerization in aqueous solution. However, studies on their behavior in extraction processes are scarce. This paper addressed the issue by considering five commonly used extraction processes. Unlike dynamic maceration (DM) and ultrasound-assisted extraction, substantial isomerization was induced by static maceration, turbo-extraction and reflux extraction. After heating under reflux in DM, the kinetic order of isomerization was established and equations were fitted successfully using a four-parameter Weibull model (R² > 0.999). Different isomerization rates and equilibrium constants were verified, revealing a possible matrix effect on alkaloid isomerization.

Kinetic modeling of the biosorption of Cd2+ ions from aqueous solutions onto Eichhornia crassipes roots using potentiometry: low-cost alternative to conventional methods

This work presents the use of potentiometric measurements for kinetic studies of biosorption of Cd2+ ions from aqueous solutions on Eichhornia crassipes roots. The open circuit potential of the Cd/Cd2+ electrode of the first kind was measured during the bioadsorption process. The amount of Cd2+ ions accumulated was determined in real time. The data were fit to different models, with the pseudo-second-order model proving to be the best in describing the data. The advantages and limitations of the methodology proposed relative to the traditional method are discussed.

Transdermal formulations containing human sexual steroids: development and validation of methods and in vitro drug release

In vitro release of bioidentical hormones in four different liposomal transdermal emulsions (containing testosterone, progesterone, estradiol, or estradiol and estriol) was assessed. For this purpose, novel high-performance liquid chromatography methods were developed and validated in an eco-friendly manner and used to determine the in vitro release of such products. The methods were suitable for our intended goal, and the emulsions employed were found to be effective as transporting candidates for the efficient release of hormones in the transdermal delivery of human sexual steroids.

Optimization of chromatographic conditions and comparison of extraction efficiencies of four different methods for determination and quantification of pesticide content in bovine milk by UFLC-MS/MS

This paper describes the optimization of a multiresidue chromatographic analysis for the identification and quantification of 20 pesticides in bovine milk, including three carbamates, a carbamate oxime, six organophosphates, two strobilurins, a pyrethroid, an oxazolidinedione, an aryloxyphenoxypropionate acid/ester, a neonicotinoid, a dicarboximide, and three triazoles. The influences of different chromatographic columns and gradients were evaluated. Furthermore, four different extraction methods were evaluated; each utilized both different solvents, including ethyl acetate, methanol, and acetonitrile, and different workup steps. The best results were obtained by a modified QuEChERS method that lacked a workup step, and that included freezing the sample for 2 hours at -20 ºC. The results were satisfactory, yielding coefficients of variation of less than 20%, with the exception of the 50 µg L-1 sample of famoxadone, and recoveries between 70 and 120%, with the exception of acephate and bifenthrin; however, both analytes exhibited coefficients of variation of less than 20%.

VIS-NIR SPECTROMETRY, SOIL PHOSPHATE EXTRACTION METHODS AND INTERACTIONS OF SOIL ATTRIBUTES

The objective of this study was to evaluate the relationships between the spectra in the Vis-NIR range and the soil P concentrations obtained from the PM and Prem extraction methods as well as the effects of these relationships on the construction of models predicting P concentration in Oxisols. Soil samples' spectra and their PM and Prem extraction solutions were determined for the Vis-NIR region between 400 and 2500 nm. Mineralogy and/or organic matter content act as primary attributes allowing correlation of these soil phosphorus fractions with the spectra, mainly at wavelengths between 450-550, 900-1100 nm, near 1400 nm and between 2200-2300 nm. However, the regression models generated were not suitable for quantitative phosphate analysis. Solubilization of organic matter and reactions during the PM extraction process hindered correlations between the spectra and these P soil fractions. For Prem,, the presence of Ca in the extractant and preferential adsorption by gibbsite and iron oxides, particularly goethite, obscured correlations with the spectra.

SIMULTANEOUS DETERMINATION OF PROTOCATECHUIC ALDEHYDE AND PROTOCATECHUIC ACID USING THE LOCALIZED SURFACE PLASMON RESONANCE PEAK OF SILVER NANOPARTICLES AND CHEMOMETRIC METHODS

A simple and sensitive spectrophotometric method is proposed for the simultaneous determination of protocatechuic acid and protocatechuic aldehyde. The method is based on the difference in the kinetic rates of the reactions of analytes with [Ag(NH3)2]+ in the presence of polyvinylpyrrolidone to produce silver nanoparticles. The data obtained were processed by chemometric methods using principal component analysis artificial neural network and partial least squares. Excellent linearity was obtained in the concentration ranges of 1.23-58.56 µg mL-1 and 0.08-30.39 µg mL-1 for PAC and PAH, respectively. The limits of detection for PAC and PAH were 0.039 and 0.025 µg mL-1, respectively.

MÉTODOS DE EXTRAÇÃO DE POLI-HIDROXIALCANOATOS A PARTIR DE BIOMASSA BACTERIANA

Polyhydroxyalkanoates (PHAs) are biodegradable and biocompatible polyesters intracellularly accumulated by many bacteria as an energy reserve material and carbon source. These biopolymers may be extracted from cells after their production phase, and the extraction process involves various individual operations to ensure adequate removal of the biopolymer from the cells. During this process, the following aspects should be considered: reduction of product losses during different stages of the process to obtain a highly pure product, preservation of physical and thermal characteristics, and use of low toxicity chemicals to achieve sustainable production and avoid harming the environment. The impact of the costs of PHA extraction on the total cost of the production process may account for over 50% of the end-value of the product. Within this context, several methods of PHA extraction have been reported in the literature. These methods include the use of solvents, chemical digestion, enzymatic digestion, mechanical extraction with high-pressure homogenization and ultrasound, extraction using supercritical fluids, or a combination of these methods. The present review of the literature shows strategies for extraction processes of PHAs produced by bacteria involving cell destabilization and/or breakage, recovery, and purification of the biopolymer.