High-performance Liquid Chromatography Measurements Research Articles

Physical-chemical measurement method development for self-assembled, core-shell nanoparticles

Improvements in dimensional metrology and innovations in physical-chemical characterization of functionalized nanoparticles are critically important for the realization of enhanced performance and benefits of nanomaterials. Toward this goal, we propose a multi-technique measurement approach, in which correlated atomic force microscopy, dynamic light scattering, high performance liquid chromatography and mass spectroscopy measurements are used to assess molecular and structural properties of self-assembled polyplex nanoparticles with a core-shell structure. In this approach, measurement methods are first validated with a model system consisting of gold nanoparticles functionalized with synthetic polycationic branched polyethylenimine macromolecules. Shell thickness is measured by atomic force microscopy and dynamic light scattering, and the polyelectrolyte uptake determined by chromatographic separation and mass spectrometric analysis. Statistical correlation between size, structure and stability provide a basis for extending the methods to more complex self-assembly of nucleic acids and macromolecules via a condensation reaction. From these size and analytical chemical measurements, we obtain a comprehensive spatial description of these assemblies, obtain a detailed interpretation of the core-shell evolution, and identify regions of the parameter space where stable, discrete particle formation occurs.

Solar light-driven complete mineralization of aqueous gram-positive and gram-negative bacteria with ZnO photocatalyst

ZnO nanoparticles have been effectively used in water disinfection from two common types of gram-positive (Enterococcus faecium) and gram–negative (Proteus mirabilis) bacteria under simulated solar radiations by inactivation. Complete mineralization of organic contents that leach out of inactivated bacteria has also been achieved leaving no soluble organic matter in water. Bacterial inactivation and complete mineralization have been confirmed by plate counting, high performance liquid chromatography and total organic content measurement. Effects of different reaction parameters (pH, temperature, bacterial concentration, reaction time and ZnO catalyst loading) have all been studied. Control experiments with Cut-off filters confirm the role of the UV tail in solar simulated light in the photocatalytic process. The results highlight the feasibility of using ZnO photocatalyst in complete disinfection of water from both hazardous Enterococcus and Proteus mirabilis bacteria, leaving no organic matters after degradation.

Highly efficient modified lead oxide electrode using a spin coating/electrodeposition mode on titanium for electrochemical treatment of pharmaceutical pollutant

In this study, Ti/TiO2/PbO2 anodes consisting of a PbO2 coating growth on the TiO2 interlayer deposited on titanium substrates were prepared combining different deposition technics: electrochemical method using anodization (Anod), electrodeposition (EL), and sol gel spin coating (SG). Different kinds of anodes have been tested for the removal of ampicillin, a pharmaceutical pollutant, from water. The structure and the surface morphology of the prepared multiple coatings were characterized by scanning electron microscopy and Energy-Dispersive X-ray spectroscopy respectively. Electrochemical impedance spectroscopy was also investigated in order to study the electrocatalytic activity of the anodes. The performance of the electrodes was evaluated through high performance liquid chromatography and chemical oxygen demand (COD) measurements. It was noticed that ampicillin could be mineralized by anodic oxidation process using Ti/TiO2/PbO2 anodes. The best results were obtained for Ti/TiO2SG/PbO2EL as anode with a 64% of COD removal after 300 min of treatment and a fast decrease in the amount of ampicillin was reached after almost one hour. Experimental results demonstrate that Ti/TiO2SG/PbO2EL anode presents the best ability for the degradation of ampicillin through anodic oxidation compared to the Ti/TiO2SG/PbO2SG and Ti/TiO2Anod/PbO2EL electrodes.

Properties of PMMA Bone Cement Modified with Nano-hydroxyapatite and Acetone

Fracture in the adjacent levels is one of the consequences to the use of commercial poly methylmethacrylate (PMMA) bone cement. Modified PMMA with a reduced Young’s modulus was found to be safer for cancellous bone augmentation procedures. The aim of this research was to study the effect of adding hydroxyapatite (HA) nano-particles and acetone on different properties of PMMA cement. A commercial PMMA cement was used as a model for bone cement. Three groups of modified PMMA/nano-HA were investigated by adding 2, 4 and 6 wt. % of HA. Acetone as a porogen mixed with distilled water in different amounts (A/W: 1:1, 2:1.5 and 2:1g) was used to produce porous PMMA cement. The residual monomer, polymerization and mechanical properties under tension and compression tests were investigated. Young’s modulus detected from compression test decreased from 826.5±10 to 728±66 MPa by adding 6wt.% HA. Adding acetone to PMMA with 2:1.5g (A/W) has decreased the compressive Young’s modulus to 753±38 MPa. High Performance Liquid Chromatography (HPLC) measurements were carried out with intervals of 2 hours, 6 hours and 24 hours to evaluate the residual monomer for all groups. The amount of residual monomer has decreased after 24 hours of curing by adding acetone and nano-HA. Modifying PMMA by HA and acetone have inconsistent effect on the polymerization temperature. It was concluded that HA and acetone can be used to reduce the stiffness and residual monomer with enhanced biocompatibility of the commercial PMMA bone cement.

Concentrations of Multiple Phytoplankton Pigments in the Global Oceans Obtained from Satellite Ocean Color Measurements with MERIS

The remote sensing of chlorophyll a concentration from ocean color satellites has been an essential variable quantifying phytoplankton in the past decades, yet estimation of accessory pigments from ocean color remote sensing data has remained largely elusive. In this study, we validated the concentrations of multiple pigments (Cpigs) retrieved from in situ and MEdium Resolution Imaging Spectrometer (MERIS) measured remote sensing reflectance (Rrs(λ)) in the global oceans. A multi-pigment inversion model (MuPI) was used to semi-analytically retrieve Cpigs from Rrs(λ). With a set of globally optimized parameters, the accuracy of the retrievals obtained with MuPI is quite promising. Compared with High-Performance Liquid Chromatography (HPLC) measurements near Bermuda, the concentrations of chlorophyll a, b, c ([Chl-a], [Chl-b], [Chl-c]), photoprotective carotenoids ([PPC]), and photosynthetic carotenoids ([PSC]) can be retrieved from MERIS data with a mean unbiased absolute percentage difference of 38%, 78%, 65%, 36%, and 47%, respectively. The advantage of the MuPI approach is the simultaneous retrievals of [Chl-a] and the accessory pigments [Chl-b], [Chl-c], [PPC], [PSC] from MERIS Rrs(λ) based on a closure between the input and output Rrs(λ) spectra. These results can greatly expand scientific studies of ocean biology and biogeochemistry of the global oceans that are not possible when the only available information is [Chl-a].

Complexes of the Mycotoxins Citrinin and Ochratoxin A with Aluminum Ions and their Spectroscopic Properties.

The sensitive detection of the mycotoxin citrinin (CIT) utilizing its fluorescence requires approaches to enhance the emission. In this respect, we studied the complexation of CIT and ochratoxin A (OTA) with Al3+ in methanol using absorption and fluorescence spectroscopy. In this context, an isocratic high performance liquid chromatography (HPLC) method using a polymer column and a fluorescence detector was also developed that enables the separation of the metal ion complexes from the free ligands and non-complexed Al3+. CIT and OTA showed distinct changes in their absorption and fluorescence properties upon Al3+-coordination, and the fluorescence of CIT was considerably enhanced. Analysis of the photometrically assessed titration of CIT and OTA with Al3+ using the Job plot method revealed 1:2 and 1:1 stoichiometries for the Al3+ complexes of CIT (Al:CIT) and OTA (Al:OTA), respectively. In the case of CIT, only one β-diketone moiety participates in Al3+ coordination. These findings can be elegantly exploited for signal amplification and provide the base to reduce the limit of detection for CIT quantification by about an order of magnitude, as revealed by HPLC measurements using a fluorescence detector.

Synthesis and characterization of La-doped Zn(O,S) photocatalyst for green chemical detoxification of 4-nitrophenol.

La-doped Zn(O,S) nanoparticles (NPs) with different contents of lanthanum have been synthesized with a simple sol-gel method at low temperature (90 ℃) for 4-nitrophenol (4-NP) detoxification. The as-prepared catalysts were characterized with X-ray diffraction (XRD), scanning electron microscope (SEM), high resolution transmission electron microscope (HRTEM), photoluminescence (PL) and UV-vis absorbance spectroscopy, X-ray photoelectron spectroscopy (XPS), electrochemical impedance spectroscopy (EIS), and photoresponsivity. In this work, it is considered that the detoxification of 4-NP to 4-aminophenol (4-AP) without NaBH4 by using photocatalytic method is a green chemical conversion. The experimental data showed 30 ppm toxic 4-NP had been totally converted to useful 4-aminophenol (4-AP) with lower toxicity in 2 h, which was confirmed with a specific peak shift as indicated with UV-vis absorbance spectra and high performance liquid chromatography (HPLC) measurement. The lower amount of evolved hydrogen from photocatalytic process on La-doped Zn(O,S) NPs in the presence of 4-NP confirmed the produced hydrogen was consumed as a reducing agent during the 4-NP-to-4-AP conversion. The photocatalytic detoxification of 4-NP to 4-AP had been demonstrated and an appropriate mechanism based on the experimental data had been proposed and elucidated in this work.

A High-performance Liquid Chromatography Measurement of Kynurenine and Kynurenic Acid: Relating Biochemistry to Cognition and Sleep in Rats

The kynurenine pathway (KP) of tryptophan degradation has been implicated in psychiatric disorders. Specifically, the astrocyte-derived metabolite kynurenic acid (KYNA), an antagonist at both N-methyl-d-aspartate (NMDA) and α7 nicotinic acetylcholine (α7nACh) receptors, has been implicated in cognitive processes in health and disease. As KYNA levels are elevated in the brains of patients with schizophrenia, a malfunction at the glutamatergic and cholinergic receptors is believed to be causally related to cognitive dysfunction, a core domain of the psychopathology of the illness. KYNA may play a pathophysiologically significant role in individuals with schizophrenia. It is possible to elevate endogenous KYNA in the rodent brain by treating animals with the direct bioprecursor kynurenine, and preclinical studies in rats have demonstrated that acute elevations in KYNA may impact their learning and memory processes. The current protocol describes this experimental approach in detail and combines a) a biochemical analysis of blood kynurenine levels and brain KYNA formation (using high-performance liquid chromatography), b) behavioral testing to probe the hippocampal-dependent contextual memory (passive avoidance paradigm), and c) an assessment of sleep-wake behavior [telemetric recordings combining electroencephalogram (EEG) and electromyogram (EMG) signals] in rats. Taken together, a relationship between elevated KYNA, sleep, and cognition is studied, and this protocol describes in detail an experimental approach to understanding function outcomes of kynurenine elevation and KYNA formation in vivo in rats. Results obtained through variations of this protocol will test the hypothesis that the KP and KYNA serve pivotal roles in modulating sleep and cognition in health and disease states.

A High-performance Liquid Chromatography Measurement of Kynurenine and Kynurenic Acid: Relating Biochemistry to Cognition and Sleep in Rats

A High-performance Liquid Chromatography Measurement of Kynurenine and Kynurenic Acid: Relating Biochemistry to Cognition and Sleep in Rats

Mesoporous silica microparticles gated with a bulky azo derivative for the controlled release of dyes/drugs in colon.

Mesoporous silica microparticles were prepared, loaded with the dye safranin O (M-Saf) or with the drug budesonide (M-Bud) and capped by the grafting of a bulky azo derivative. Cargo release from M-Saf at different pH values (mimicking those found in the gastrointestinal tract) in the absence or presence of sodium dithionite (a reducing agent mimicking azoreductase enzyme present in the colon) was tested. Negligible safranin O release was observed at pH 6.8 and 4.5, whereas a moderate delivery at pH 1.2 was noted and attributed to the hydrolysis of the urea bond that linked the azo derivative onto the external surface of the inorganic scaffold. Moreover, a marked release was observed when sodium dithionite was present and was ascribed to the rupture of the azo bond in the molecular gate. Budesonide release from M-Bud in the presence of sodium dithionite was also assessed by ultraviolet-visible spectroscopy and high performance liquid chromatography measurements. In addition, preliminary in vivo experiments with M-Saf carried out in mice indicated that the chemical integrity of the microparticles remained unaltered in the stomach and the small intestine, and safranin O seemed to be released in the colon.

HappyTools: A software for high-throughput HPLC data processing and quantitation.

High-performance liquid chromatography (HPLC) is widely used for absolute quantitation. The advent of new columns and HPLC technology has enabled higher sample throughput, and hence, larger scale studies that perform quantitation on different sample types (e.g. healthy controls vs. patients with rheumatoid arthritis) using HPLC are becoming feasible. However, there remains a lack of methods that can analyse the increased number of HPLC samples. To address this in part, the modular toolkit HappyTools has been developed for the high-throughput targeted quantitation of HPLC measurements. HappyTools enables the user to create an automated workflow that includes retention time (tr) calibration, data extraction and the calculation of several quality criteria for data curation. HappyTools has been tested on a biopharmaceutical standard and previously published clinical samples. The results show comparable accuracy between HappyTools, Waters Empower and ThermoFisher Chromeleon. However, HappyTools offered superior precision and throughput when compared with Waters Empower and ThermoFisher Chromeleon. HappyTools is released under the Apache 2.0 license, both the source code and a Windows binary can be freely downloaded from https://github.com/Tarskin/HappyTools.

Solubilisation behaviour of poorly water-soluble drugs during digestion of solid SMEDDS

Lipid based-formulations can enhance the bioavailability of poorly water-soluble lipophilic drugs through enhanced solubilisation of drugs in the gastrointestinal (GI) tract during digestion. This study investigates the solubilisation behaviour of poorly water-soluble drugs upon digestion of solid self-microemulsifying drug delivery system (S-SMEDDS). The S-SMEDDS were prepared using two different core lipids, Gelucire® 44/14 (GEL) or glyceryl monooleate (GMO), and were loaded with two model drugs, fenofibrate (FEN) and cinnarizine (CINN). S-SMEDDS formulations were characterized using wide-angle X-ray scattering (WAXS) and Raman spectroscopy, and their structural behaviour and drug solubilisation behaviour were monitored using drug-related diffraction peaks during digestion under fasted and fed simulated intestinal conditions using time-resolved small and wide-angle X-ray scattering (SAXS/WAXS). The concentrations of FEN and CINN released into the aqueous phase (AP) during digestion were quantified using high-performance liquid chromatography (HPLC). Both model drugs, FEN and CINN, had greater solubility in the GMO-based S-SMEDDS formulations and were partially solubilised into lipid matrix and uniformly distributed in solid formulations. The extent of digestion was greater for the GEL-based systems (92–94%) than GMO-based systems (65–75%) as was the rate of digestion. GEL-based S-SMEDDS formulations formed a lamellar phase during digestion in the fasted state and formed mixed micelles in the fed state. In contrast, the GMO-based system formed the mixed micelles in both intestinal conditions. The time-resolved SAXS profiles revealed solubilisation of crystalline drugs into the lipolysis products. Synchrotron SAXS results were in correlation with the HPLC measurements, confirming the ability of the SAXS technique to monitor drug behaviour and showing that the digestion of S-SMEDDS can enhance drug solubilisation.

Hantzsch pre-column derivatization for simultaneous determination of alendronate sodium and its pharmacopoeial related impurity: Comparative study with synchronous fluorometry using fluorescamine

High performance liquid chromatographic (HPLC) method with a pre-column derivatization based on Hantzsch condensation reaction was applied for simultaneous determination of alendronate sodium (ALN) and its main related impurity, 4-Aminobutanoic acid (ABA) at its pharmacopeial limit. The separation of colored condensation products of ALN and ABA were achieved on Agilent Zobrax Eclipse SB-C18 analytical column (250 × 4.6 mm, 5 μm) using a mobile phase composed of acetonitrile–0.1 M acetate buffer, pH 5.0 (15:85, v/v). The flow rate was 1 mL min−1. The detection was carried out at 340 nm using photo-diode array detector. Peak areas were used for the linear regression line in the range of 10–500 and 0.2–40 μg mL−1 for ALN and ABA, respectively. Different conditions for the optimization of the derivatization reactions as well as for the HPLC measurement were studied. The proposed method was validated for linearity, precision, accuracy, specificity and robustness. This method was used to check the purity of ALN in the presence of ABA (related impurity) at the pharmacopeial limit (0.5%). For comparison purpose, another method was proposed which involves synchronous fluorescence measurement after ALN reaction with fluorescamine. In this method, the third derivative synchronous spectra were estimated as peak to peak measurement from 339 to 370 nm for ALN determination with LOD and LOQ of 24 and 73 ng mL−1, respectively, showing very high sensitivity. Both methods have been applied for determination of the alendronate sodium (ALN) in bulk and pharmaceutical preparations without interference of additives in tablets or oral solution.

Immune-unreactive urinary albumin as a predictor of cardiovascular events: the Hortega Study.

We aimed to determine if immune-unreactive albumin excretion (IURAE) is associated with cardiovascular (CV) events in a representative sample of a general population from Spain. We included 1297 subjects (mean age ± standard error 48.0 ± 0.2 years, 48% females), who participated in the Hortega Follow-Up Study. The primary endpoint was incidence of fatal and non-fatal CV events. Urinary albumin excretion (UAE) was measured in spot voided urine, frozen at -80°C, by immunonephelometry [immune-reactive albumin excretion (IRAE)] and by high-performance liquid chromatography (HPLC) [total albumin excretion (AE)]. IURAE was calculated as the difference between HPLC measurements and IRAE. We estimated fully adjusted hazard ratios (HRs) of CV incidence by Cox regression for IRAE, IURAE and total AE. After an average at-risk follow-up of 13 years, we observed 172 CV events. urinary albumin to creatinine ratio (UACR) of ≥30 mg/g assessed by IRAE, IURAE or total AE concentrations was observed in 74, 273 and 417 participants, respectively. Among discordant pairs, there were 49 events in those classified as micro- and macroalbuminuric by IURAE, but normoalbuminuric by IRAE. Only the IRAE was a significant independent factor for the incidence of CV events [HR (95% confidence interval) 1.15 (1.04-1.27)]. The association of UAE with CV events was mainly driven by heart failure (HF) [HR 1.33 (1.15-1.55) for IRAE; HR 1.38 (1.06-1.79) for IURAE; HR 1.62 (1.22-2.13) for total AE]. Those subjects who were micro- and macroalbuminuric by both IRAE and IURAE had a significant increase in risk for any CV event, and especially for HF. IRAE, IURAE and AE were associated with an increased risk for CV events, but IRAE offered better prognostic assessment.

Building a database for brain 18 kDa translocator protein imaged using [11C]PBR28 in healthy subjects

Translocator protein 18 kDa (TSPO) has been widely imaged as a marker of neuroinflammation using several radioligands, including [11C]PBR28. In order to study the effects of age, sex, and obesity on TSPO binding and to determine whether this binding can be accurately assessed using fewer radio high-performance liquid chromatography (radio-HPLC) measurements of arterial blood samples, we created a database of 48 healthy subjects who had undergone [11C]PBR28 scans (23 high-affinity binders (HABs) and 25 mixed-affinity binders (MABs), 20 F/28 M, age: 40.6 ± 16.8 years). After analysis by Logan plot using 23 metabolite-corrected arterial samples, total distribution volume (VT) was found to be 1.2-fold higher in HABs across all brain regions. Additionally, the polymorphism plot estimated nondisplaceable uptake (VND) as 1.40 mL · cm−3, which generated a specific-to-nondisplaceable ratio (BPND) of 1.6 ± 0.6 in HABs and 1.1 ± 0.6 in MABs. VT increased significantly with age in nearly all regions and was well estimated with radio-HPLC measurements from six arterial samples. However, VT did not correlate with body mass index and was not affected by sex. These results underscore which patient characteristics should be accounted for during [11C]PBR28 studies and suggest ways to perform such studies more easily and with fewer blood samples.

P.2.026 - No tolerance to anticompulsive activity of trace amine-associated receptor 1 agonist following repeated administration

Introduction In clinical practice the treatment of psychiatric diseases usually requires long-term drug administration, but the effects of many psychiatric medications decrease upon repeated exposure, a phenomenon described as ‘tolerance’ [1]. Our previous study has shown that acute administration of partial Trace Amine-Associated Receptor 1 (TAAR1) agonist (RO5263397) attenuated adjunctive water drinking in schedule-induced polydipsia (SIP) [2], a successful model of compulsive behavior [3]. The present study was aimed to evaluate the anticompulsive activity of RO5263397 following repeated administration and analyze RO5263397 effects on the levels of monoamines and their metabolites in the striatum and frontal cortex. Methods To induce SIP, 16 Wistar rats were habituated to operant chambers and pellet feeding to fixed-time 60-second (FT-60 sec) schedule of food-pellet reinforcement. After the acquisition of stable adjunctive drinking behaviour, the animals were divided into two equal subgroups. The different subgroups were injected with either 12 mg/kg of RO5263397 or vehicle every 12 hours (9:00 and 21:00) during 7 consecutive days. The drug dose and the schedule of injections were chosen in concordance with a previously published information about pharmacokinetic of RO5263397 [4]. Thus, the serum concentration of RO5263397 was higher than 0.67 μg/ml (maximal concentration after i.p. administration of RO5263397 in dose 3 mg/kg which decreased SIP in our previous experiments [2]) for 14 hours in a day. To analyze monoamines tissue content high-performance liquid chromatography (HPLC) was used. HPLC measurements were carried out as described before [5]. Striatum and frontal cortex tissues were dissected from the rats subchronically treated with RO5263397 and levels of norepinephrine, dopamine, serotonin and their metabolites were evaluated. Results Before the start of the treatment there was no difference between the subgroups in water consumption in home cages and operant boxes (U-tests, Ps>0.05). Two-way repeated measures ANOVA showed that the treatment with RO5263397 significantly reduced SIP (F(1.13)=17.865, P At the same time, repeated treatment with RO5263397 significantly decreased dopamine metabolism and increased norepinephrine and serotonin levels in the striatum and prefrontal cortex (with exception of norepinephrine) (t- and U-tests, Ps Conclusions Thus, these findings indicate that the repeated administration did not influence SIP ameliorating effect of RO5263397 and further support previously proposed view that TAAR1 is promising target for the treatment of disorders accompanied by compulsive behavior. Moreover, HPLC results suggest that the mechanisms of the TAAR1 agonist anticompulsive activity might involve the modulation of not only dopamine but also other catecholamine systems. Certainly, additional studies aimed at analysis of neurochemical profile of activity of TAAR1 agonists are warranted.

Pt‐Sn‐Eu/C Catalysts: Application of Rare Earth Metals as Anodes in Direct Ethanol Fuel Cells

AbstractPt‐Sn‐Eu catalysts were synthesized by modified polyol method, evaluated for the ethanol oxidation reaction (EOR), and compared to commercial Pt/C and Pt‐Sn/C catalysts. The catalysts were electrochemically characterized in both three‐electrode and fuel cell setups. X‐ray diffraction measurements indicated some degree of Pt‐Sn alloying in the Pt‐Sn‐Eu/C catalysts, and mean crystallite sizes between 2.3–3.3 nm, while X‐ray photoelectron spectroscopy measurements showed the presence of Pt and Sn in both metallic and oxide form, and rare earth metals in the form of mixed oxides. Adding tin and europium promoted filling of the Pt 5d band, as confirmed by X‐ray absorption. The electrochemical characterization showed a higher oxidation current density and lower oxidation onset potential for the ternary Pt‐Sn‐Eu materials compared with the commercial catalysts, in both the three‐cell and fuel cell tests. High performance liquid chromatography measurements indicating that the main products of ethanol oxidation were acetaldehyde and acetic acid; a low concentration of CO2 was also detected. The improved ethanol oxidation efficiency for the Pt‐Sn‐Eu/C catalysts can be explained by the Sn/Eu‐Pt electronic effect, because it weakens the adsorption of intermediate products by Pt, and favors the bifunctional EOR mechanism, as europium oxide renders oxygenated species available at lower potentials.

Destruction of chemical warfare surrogates using a portable atmospheric pressure plasma jet

Today’s reality is connected with mitigation of threats from the new chemical and biological warfare agents. A novel investigation of cold plasmas in contact with liquids presented in this paper demonstrated that the chemically reactive environment produced by atmospheric pressure plasma jet (APPJ) is potentially capable of rapid destruction of chemical warfare agents in a broad spectrum. The decontamination of three different chemical warfare agent surrogates dissolved in liquid is investigated by using an easily transportable APPJ. The jet is powered by a kHz signal source connected to a low-voltage DC source and with He as working gas. The detailed investigation of electrical properties is performed for various plasmas at different distances from the sample. The measurements of plasma properties in situ are supported by the optical spectrometry measurements, whereas the high performance liquid chromatography measurements before and after the treatment of aqueous solutions of Malathion, Fenitrothion and Dimethyl Methylphosphonate. These solutions are used to evaluate destruction and its efficiency for specific neural agent simulants. The particular removal rates are found to be from 56% up to 96% during 10 min treatment. The data obtained provide basis to evaluate APPJ’s efficiency at different operating conditions. The presented results are promising and could be improved with different operating conditions and optimization of the decontamination process.

Influence of Environmental and Microclimate Factors on the Coffee Beans Quality (C. canephora): Correlation between Chemical Analysis and Stable Free Radicals

The present study reports a physicochemical comparison of shade-grown and sun-grown coffee beans, under unripe, rip and roasted-ripe conditions, using electrical conductivity measurements, electron paramagnetic resonance (EPR), infrared spectroscopy (FTIR), and high performance liquid chromatography (HPLC). Moreover, the assessed physicochemical parameters were compared with organoleptic evaluations based on the Coffee Quality Institute protocol. The values found for electrical conductivity, leached potassium, and stable free radicals were respectively 29%, 31%, and 350% higher for shade-grown coffee beans, whereas polyphenol oxidase enzymatic activity was 23% lower. By contrast, FTIR and HPLC measurements identified higher chlorogenic acid and lipid contents in sun-grown coffee beans. Importantly, the sensorial grade attributed to roasted-ripe grains was 12% higher for sun-grown coffee. Our findings suggest that shade-grown coffee beans have undergone microorganismal activity and undesired fermentation during cultivation, which resulted in lower coffee quality. A correlation between a set of selected physicochemical properties and organoleptic properties was robustly established and could be used in the development of future coffee bean quality control protocols.

Pharmacokinetics and tissue distribution of pefloxacin mesylate in chickens.

A specific, sensitive and stable high-performance liquid chromatography (HPLC)-based analytical method was established to determine the level of pefloxacin mesylate (PM) in the plasma and various tissues of chickens. Chickens were randomly assigned to 12 equal experiment groups, including 11 treatment groups and one control group. The chickens in the treatment groups received oral administration of PM and were sacrificed at different pre-determined time points, with their blood and various organs harvested, extracted and analyzed by HPLC to quantify the level of the residual antibiotic. Method validation studies indicated that the HPLC measurement showed excellent precision, reproducibility, stability and robustness. The obtained pharmacokinetic parameters suggested that PM reached peak levels in various tissues within 1-2 h after its oral administration, and was mainly concentrated in liver and kidney. The antibiotic was also found to be cleared from chicken crureus, brain, testes, ovaries and pancreas at higher rates compared with other organs. Overall, the rapid accumulation of PM could at least be partially attributed to its relatively slow organ clearance. These results could serve as a useful guidance for the rational use of PM and other quinolone-derived antimicrobials in the treatment of infectious diseases in chickens and other animals.