Vortex-assisted microextraction of melamine from milk samples using green short chain ionic liquid solvents coupled with high performance liquid chromatography determination.

Melamine is added illegally to milk and dairy products to increase the amount of apparent protein. This organic nitrogen rich chemical compound has been of great challenge in food safety based on its adverse effect on health. Therefore, the extraction and determination of melamine from milk is necessary. Recently, ionic liquid (ILs) as solvent usage has been noticeable for low melting point, low toxicity, high thermal stability, and high extraction capabilities in a wide range of separation processes. ILs are introduced as organic-inorganic salts and green solvents in microextraction preparation. Therefore, in this study, three ionic liquids ([C6mim][NTF2], [C4mim][NTF2] and [C2mim][NTF2] ILs) were prepared and employed as an extraction solvent in dispersive liquid-liquid microextraction (DLLME) of melamine from milk samples followed by HPLC-UV. The selected ILs were designed using three types of alkyl-imidazolium (as the short organic cations) and bis (tri fluoro methyl sulfonyl) imide as anion and characterized by ATR-FTIR spectra, carbon, and hydrogen Nuclear Magnetic Resonance spectroscopy (H&C-NMR) and energy-dispersive X-ray spectroscopy (EDX). These techniques confirmed the formation of functional groups, the structure of hydrogen and carbon atoms, and various elements of ionic bond between imidazolium and bis (tri fluoro methyl sulfonyl) imide. In the next step, the effect of significant parameters, including type and volume of ILs, adsorption time, pH of the sample solution, and sample volume, were optimized. Under the optimal conditions, the limits of detection (LOD), limits of quantification (LOQ), and linearity range were obtained 63.64 µg kg-1, 210.03 µg kg-1, and 210.03-1000 µg kg-1, respectively, for as prepared [C6mim][NTF2] as the best ILs. Notably, the achieved LOQ was lower than the maximum residue level (MRL) for the melamine residue in dairy products. Eventually, the proposed method was applied to detect melamine in milk samples, and the relative recoveries were examined as 79.6-105.0 %.

Bioassay-guided isolation in Salvia abrotanoides Karel. stem based on its anti-fungal and anti-trichomonas activity.

Background and purpose: Salvia abrotanoides is considered a medicinal plant and has a broad distribution in Iran. In Iran's traditional medicine, it is also used to treat leishmaniasis, malaria, atherosclerosis, cardiovascular disease, and as a disinfectant. This research aimed to determine the anti-Candida component from S. abratonoides and anti-Trichomonas natural compounds from the stems of this plant. Experimental approach: The plant shoots were collected, dried, and after removing the leaves, grounded. Dried plant material was extracted in a maceration tank, concentrated by a Rotavap, degreased, and fractionated by normal column chromatography. Based on anti-fungal screening against Candida species, Fr. 4, with more anti-fungal activity, was selected for phytochemical analysis, by different chromatographic methods on the silica gel column and Sephadex LH-20. Isolated compounds were elucidated by NMR analysis, mass spectrum, and ultraviolet spectroscopy. Anti-fungal effects were investigated using the fungal suspension, incubation, and parasite-counting methods on purified compounds. Antibacterial effects were assessed using the Broth dilution test and reported according to the MIC parameter. Findings/Results: Two diterpenoid compounds named carnosol (compound 1), 11-hydroxy-12-methoxy-20-norabiata-8, 11, 13-trien (compound 2), and a flavonoid: 6,7-dimethoxy-5, 4'-dihydroxyflavone (compound 3) were isolated and identified. Compound 1 had selective anti-fungal effects against C. albicans, C. glabrata, and C. parapsilosis, but weak toxicity against Trichomonas vaginalis with IC50 of 675.8 µg/mL, less than metronidazole with an IC50 of 13.2 µg/mL. Conclusion and implications: Carnosol as the main component was assayed against Candida, Aspergillus, Rhizopus, and Trichomanas species. The results confirmed its effect on Candida compared to standard drugs.

Magnetic silica nanoparticles adorned with a metal-organic framework; a novel nanosorbent for elimination of aqueous Pb ions contaminant.

The annual growth of water pollution resulting from the uncontrolled entry of heavy metals, like Pb2+ ions, is one of the most critical global concerns due to its direct and indirect effects on human life. The absorption of this component by the body could affect the nervous system via oxidative stress production or disturbing cellular biological mechanism. So, it is important to find an effective method for purifying the existing waters. This study aims to fabricate and compare the effect of two new nano-adsorbents (Fe3O4@ZIF-8 and Fe3O4@SiO2@ZIF-8) on removing Pb2+ ions from the aqueous solution. Accordingly, iron oxide nanoparticles were synthesized via co-precipitation method at first and then coated with a silica shell through the sol-gel method. Both nanoparticles were coated with a layer of metal-organic framework (MOF), ZIF-8, and analyzed with different physicochemical tests. In the following parts, the Pb2+ ion removal capability of the nano-adsorbents was evaluated in the presence of different parameters, including nanosorbent concentrations, contact time, pH, and pollutant concentrations. Results confirmed preparation of nanoparticles with a mean size of about 110 ± 10 nm and 80 ± 10 nm for Fe3O4@ZIF-8 and Fe3O4@SiO2@ZIF-8, respectively. Both nanoparticles showed the highest amount of pollutants removal (near 90% for both nanoparticles) at pH = 6 within 15 min of contact in the presence of 100 ppm Pb2+ ions. Besides, in the case of real samples, with a concentration of about 150 ppm of Pb2+ ions, they showed maximum adsorption of about 93.61% and 99.2% for Fe3O4@ZIF-8 and Fe3O4@SiO2@ZIF-8, respectively. The presence of iron oxide nanoparticles in the structure of this adsorbent makes it easy to separate them in a user-friendly method. A brief comparison between these nanosorbents indicates that Fe3O4@SiO2@ZIF-8 nanoparticles have better performance due to their higher porosity and surface area ratio and so it could be used as a cost-effective ideal nanosorbent candidate for easy removal of heavy metals from water.

Dietary Thymol Improved Growth, Body Composition, Digestive Enzyme Activities, Hematology, Immunity, Antioxidant Defense, and Resistance to Streptococcus iniae in the Rainbow Trout (Oncorhynchus mykiss).

In this study, thymol (TYM) at dietary levels of 0, 1, 1.5, 2, and 2.5 g/kg diet was used to evaluate its effects on growth, digestive performance, immunity, and resistances to the infection induced by Streptococcus iniae in the rainbow trout, Oncorhynchus mykiss. A number of 450 fish (35.8 ± 4.4 g; Mean ± SD) were distributed to 15 tanks (30 fish/tank) in three replicates and fed TYM for 60 days. After feeding period, Fish fed 1.5-2.5 g TYM showed better growth, higher digestive enzyme activity, and body protein content compared to other diets (P < 0.05). Regression analysis indicated a polynomial relationship between growth parameters and dietary TYM levels. Based upon the varied growth parameters, the optimum dietary TYM level was 1.89% for FCR. TYM at dietary levels of 1.5-2.5 g significantly enhanced liver antioxidant enzyme activity [superoxide dismutase (SOD), glutathione peroxidase (GPx), and catalase (CAT)], immune components in blood [alternative complement activity (C3), total immunoglobulin (Ig), lysozyme activity, bactericidal activity, and total protein], and in mucus [alkaline phosphatase (ALP), protease activity, lysozyme activity, bactericidal activity, and total protein] compared to other diets (P < 0.05). TYM at dietary levels of 2-2.5 g significantly decreased malondialdehyde (MDA) levels compared to other experimental groups (P < 0.05). In addition, use of TYM at dietary levels of 1.5-2.5 g upregulated the expression of the immune-related genes (C3, Lyz, and Ig) (P < 0.05). In contrast, the expression of inflammatory genes, tumor necrosis factor (TNF-α) and Interleukin-8 (IL-8) significantly were downregulated in response to 2-2.5 g TYM (P < 0.05). The hematology of the fish also altered in response to dietary TYM, where the values of corpuscular hemoglobin concentration (MCHC), hemoglobin (Hb), red blood cell (RBC), hematocrit (Hct), and white blood cell (WBC) significantly increased in fish fed 2-2.5 g TYM compared to other diets (P < 0.05). In addition, MCV significantly decreased in response to 2-2.5 g TYM (P < 0.05). After challenge with Streptococcus iniae, the survival rate was significantly higher in fish fed 2-2.5 g TYM compared to other diets (P < 0.05). The results of the present study concluded that TYM in the diet of rainbow trout can improve the fish growth and immunity and increase the resistance of the fish to Streptococcus iniae infection. The results of this study recommend an optimized dietary level of 2-2.5 g TYM for the fish.

A review of strategies for untargeted urinary metabolomic analysis using gas chromatography-mass spectrometry.

BACKGROUND: Human urine gives evidence of the metabolism in the body and contains different metabolites at various concentrations. A number of analytical techniques including mass spectrometry (MS) and nuclear magnetic resonance (NMR) have been used to obtain metabolites levels in urine samples. However, gas chromatography-mass spectrometry (GC-MS) is one of the most widely used techniques for urinary metabolomics studies due to its higher sensitivity, resolution, reproducibility, reliability, relatively low cost and ease of operation compared to liquid chromatography-mass spectrometry and NMR. AIM OF REVIEW: This review looks at various aspects of urine preparation prior to analysis by GC-MS including sample storage, urease pretreatment, derivatization, use of internal standard and quality control samples for data correction. In addition, most common types of inlet liners, ionization techniques and columns are discussed and a summary of mass analyzers are also highlighted. Lastly, the role of retention index in metabolite identification and data normalization methods are presented. KEY SCIENTIFIC CONCEPTS OF REVIEW: The purpose of this review is summarizing methods of sample storage, pretreatment, and GC-MS analysis that are mostly used in urine metabolomics studies. Specific emphasis is given to the critical steps within the GC-MS urine metabolomics that those new to this field need to be aware of and the remaining challenges that require further attention and studies.

PCB-Based Magnetometer as a Platform for Quantification of Lateral-Flow Assays.

This work presents a proof-of-concept demonstration of a novel inductive transducer, the femtoMag, that can be integrated with a lateral-flow assay (LFA) to provide detection and quantification of molecular biomarkers. The femtoMag transducer is manufactured using a low-cost printed circuit board (PCB) technology and can be controlled by relatively inexpensive electronics. It allows rapid high-precision quantification of the number (or amount) of superparamagnetic nanoparticle reporters along the length of an LFA test strip. It has a detection limit of 10-10 emu, which is equivalent to detecting 4 ng of superparamagnetic iron oxide (Fe3O4) nanoparticles. The femtoMag was used to quantify the hCG pregnancy hormone by quantifying the number of 200 nm magnetic reporters (superparamagnetic Fe3O4 nanoparticles embedded into a polymer matrix) immuno-captured within the test line of the LFA strip. A sensitivity of 100 pg/mL has been demonstrated. Upon further design and control electronics improvements, the sensitivity is projected to be better than 10 pg/mL. Analysis suggests that an average of 109 hCG molecules are needed to specifically bind 107 nanoparticles in the test line. The ratio of the number of hCG molecules in the sample to the number of reporters in the test line increases monotonically from 20 to 500 as the hCG concentration increases from 0.1 ng/mL to 10 ng/mL. The low-cost easy-to-use femtoMag platform offers high-sensitivity/high-precision target analyte quantification and promises to bring state-of-the-art medical diagnostic tests to the point of care.

Correction: Enhancement of lateral flow assay performance by electromagnetic relocation of reporter particles.

[This corrects the article DOI: 10.1371/journal.pone.0186782.].

Designing instrumented walker to measure upper-extremity's efforts: A case study.

The high prevalence of shoulder pain in using walkers in patients who have spinal cord injury (SCI). Also, the limited options available to economically measure grip forces in walkers, which drove the need to create one. This article describes a method to obtain upper-extremities' forces and moments in a person with SCI by designing an appropriate instrumented walker. First, since the commercial multidirectional loadcells are too expensive, custom loadcells are fabricated. Ultimately, a complete gait analysis by means of VICON motion analysis and using inverse dynamic method has been held to measure upper-extremities' efforts. The results for a person with SCI using a two-wheel walker in low and high heights and a basic walker show that there are higher shoulder and elbow flexion-extension moments and also higher shoulder forces in superior-inferior direction and higher elbow and wrist forces in anterior-posterior directions. The results are not much different in using two different types of walker. By using the proposed method, upper-extremities' forces and moments were obtained and the results were compared to each other in using two different walkers.

Aptamer functionalized magnetic nanoparticles for effective extraction of ultratrace amounts of aflatoxin M1 prior its determination by HPLC.

Aptamers, due to the inherently high selectivity towards target analytes, are promising candidate for surface modification of the nanoparticles. Therefore, aptamer-functionalized magnetic nanoparticles (AMNPs) was prepared and used to develop a magnetic solid-phase extraction procedure for clean-up of milk and dairy products samples before measuring the aflatoxin M1 (AFM1) contents by the high-performance liquid chromatography. The prepared sorbent was characterized by different instrumental methods such as FT-IR, FESEM, TEM, EDX and AGFM. The AMNPs was used in extraction and pre-concentration of ultratrace amounts AFM1 from local milk samples. The amount of sorbent, elution volume, extraction time, and salt addition were optimized. Based on the results, calibration plot is linear over the 0.3 to 1 ng·L-1 and 5 to 50 ng·L-1 AFM1 concentration ranges. The limits of detection of the developed method were obtained 0.2 ng·L-1 which is the smallest value that has been reported up to now. The results show that this new superior sorbent has a large potential to simplify the complex matrix of the samples and can used for detection, preconcentration and accurate determination of ultratrace amounts of the AFM1 from milk and dairy products.

Protective effects of the prebiotic on the immunological indicators of rainbow trout (Oncorhynchus mykiss) infected with Aeromonas hydrophila.

The aim of this study was to investigate the protective effects of dietary administration of commercial prebiotic, Immunogen, on immunological indicators, enzymatic responses and stress tolerance in juvenile (81.65 ± 1.49) rainbow trout (Oncorhynchus mykiss) following Aeromonas hydrophila infection. The first group of fish was fed with the diet containing 2 g kg(-1) Immunogen whilst the control group received the diet free of Immunogen. There were three replicates per group. After 6 weeks feeding, the control group were divided into two treatments injected with saline buffer (control), and 1.5 × 10(8) CFU A. hydrophila respectively. The fish fed with the Immunogen supplemented diet were also injected with 1.5 × 10(8) CFU A. hydrophila. Our results revealed that dietary Immunogen increased the level of white blood cell (WBC) and percentage of lymphocyte (P < 0.05), however, the level of red blood cell (RBC), Hematocrit (Hct), hemoglobin (Hb) and percent of monocyte decreased in Untreated-Challenged group but unaffected in the group fed with Immunogen (P < 0.05). The level of lysozyme, alternative complement, antiprotease activity, total protein, albumin and globulin decreased in Untreated- Challenged group compared to control group. However, there was an increase in the level of lysozyme, alternative complement, antiprotease activity, bactericidal activity, in the Treated- Challenged group compared to other groups (P < 0.05). Serum alkali phosphatase (ALT) and aspartate aminotransferase, significantly increased fallowing challenge with A. hydrophila but in the Treated-Challenged group, there was no significant difference compared to the control group (P < 0.05). Lactate dehydrogenase (LDH) level was not different between groups (P > 0.05). Serum cortisol and glucose levels were higher in the challenge group, but these levels were lower in fish under challenge that were fed Immunogen-supplemented diet in contrast to the group fed control diet. The stress responses affected by A. hydrophila challenge (P < 0.05). Serum sodium, potassium and calcium concentration decreased by A. hydrophila exposure (P < 0.05), and Immunogen showed protection effect against this change.

Thermal-structural relationship of individual titania nanotubes.

The thermal properties of nano-scale materials are largely influenced by their geometry. The zero, one and quasi one dimensional forms of the same material could exhibit unique thermal transport properties depending upon the shape and nano-scale feature size. In order to gain a clear understanding of the contributions from geometrical scattering effects on thermal transport, it is required to study these nano-materials in a single isolated form rather than in clusters or films. In the past decade, titanium dioxide nanotube arrays fabricated by anodic oxidation of titanium emerged as a useful semiconductor architecture for a variety of applications, particularly for solar energy conversion. Nonetheless, the thermal properties of individual nanotubes that are important for their use in high temperature applications have not been clearly understood. Here we report the thermal transport properties of individual titania nanotubes as revealed by our preliminary study using a suspended microdevice that facilitates the thermal conductivity measurements and crystal structure investigation on the same nanotube. The nanotubes were prepared by anodic oxidation of a titanium foil in HF-DMSO electrolyte at 60 V, having outer diameters in the range of 200 to 300 nm and wall thicknesses of ∼30 to 70 nm in either amorphous or polycrystalline anatase phase. The thermal conductivity of single nanotubes was found to be very close to that of the amorphous phase (1.5 W mK(-1) and 0.85 W mK(-1) respectively) and it was only half of the thermal conductivity of the nanotube arrays in the film form. The thermal conductivity of bulk TiO2 is known to be almost six times higher. The observed thermal conductivity suppression in single nanotubes was explained using a transport model developed by considering diffuse phonon-surface scattering and scattering of phonons by ionized impurities of concentrations in the order of 10(18)-10(19) cm(-3).