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The present study reports the outcomes of assessment on acrylamide levels in selected heat-treated foods of diverse brands and origins from Saudi Arabia. In chips, acrylamide level was detected from 28 to 954 µg/kg, sample 7 (salted) contained higher amount (954 μg/kg) whereas, sample 8 (labneh and mint) comparatively produced lower amount (28 μg/kg). Nuts and dried fruits have generated acrylamide from 2 to 93 µg/kg, salted peanut of Indian origin produced higher amount (93 μg/kg) while apricot (plain) relatively generated lower amount (2 μg/kg). The levels of acrylamide in biscuits, pastry, cacao, chocolate, olive, cheese, corn, oat and wheat flakes, and bread were found from 26 to 234 µg/kg. Biscuits generated high concentration (234 μg/kg) while corn flakes fairly generated lower amount (26 μg/kg). The obtained results have shown a great variation of acrylamide content and reason might be due to foods type, cooking ingredients and, cooking methods, time and temperature.

A crucial issue in microRNA (miRNA) detection is the lack of sensitive method capable of detecting the low levels of miRNA in RNA samples. Herein, we present a sensitive and specific method for the electrocatalytic detection of miR-107 using gold-loaded nanoporous superparamagnetic iron oxide nanocubes (Au-NPFe 2 O 3 NC). The target miRNA was directly adsorbed onto the gold surfaces of Au-NPFe 2 O 3 NC via gold-RNA affinity interaction. The electrocatalytic activity of Au-NPFe 2 O 3 NC was then used for the reduction of ruthenium hexaammine(III) chloride (RuHex, [Ru(NH 3 ) 6 ] 3+ ) bound with target miRNA. The catalytic signal was further amplified by using the ferri/ferrocyanide [Fe(CN) 6 ] 3-/4- system. These multiple signal enhancement steps enable our assay to achieve the detection limit of 100aM which is several orders of magnitudes better than most of the conventional miRNA sensors. The method was also successfully applied to detect miR-107 from cancer cell lines and a panel of tissue samples derived from patients with oesophageal squamous cell carcinoma with excellent reproducibility (% RSD = < 5%, for n = 3) and high specificity. The analytical accuracy of the method was validated with a standard RT-qPCR method. We believe that our method has the high translational potential for screening miRNAs in clinical samples., (Copyright © 2017 Elsevier B.V. All rights reserved.)

A composite of multi-walled carbon nanotubes incorporated into a benzyl methacrylate-co-ethylene dimethacrylate porous monolith was prepared, characterized and used as solid phase adsorbent and as stationary phase for simultaneous extraction and separation of ten polycyclic aromatic hydrocarbons, followed by nano-liquid chromatography analysis. The extraction and chromatographic parameters were optimized with regard to the extraction efficiency and the quality of chromatographic analytes separation. Under the optimized conditions, all PAHs were separated in 13 min with suitable resolution values (Rs = 1.74-3.98). Addition of a small amount of carbon nanotubes (0.1% with respect to monomers) to the polymerization mixture increased the efficiency for the separation column to over 41,700 plates m -1 for chrysene at flow rate of 0.5 μL min -1 . The method showed a wide linear range (1-500 μg L -1 with R 2 more than 0.9938), acceptable extraction repeatability (RSDs < 6.4%, n = 3) and reproducibility (RSDs < 12.6%, five parallel-made solid phase extraction cartridges) and satisfactory detection limits (0.02-0.22 μg L -1 ). Finally, the proposed method was successfully applied to the detection of polycyclic aromatic hydrocarbons in environmental water samples. After a simple extraction procedure with preconcentration factor equal to 100, the average recovery values in ultra-pure, tap and sea water samples were found to be in the range 81.3-95.4% with %RSD less than 6.4. Again, the presence of carbon nanotubes (0.3% relatively to monomers) in native polymer enhanced the extraction performance for the solid phase adsorbent up to 78.4%. The application of the monoliths modified with CNTs in extraction and nano-scale liquid chromatography for analysis of environmental samples offered several advantages; it demonstrated an acceptable precision, low detection limits, good reproducibility, satisfying recoveries and wide dynamic linear ranges., (Copyright © 2018. Published by Elsevier B.V.)

Quantitative assessment of nitrite (NO 2 - ) anion was performed using a newly developed high throughput ultra performance liquid chromatography-mass spectrometric (UPLC-MS) method. The nitrite determination with the proposed method using micellar mobile phase was unknown. Selected ion reaction mode using negative electrospray ionization was adopted for the identification and quantitative analysis of nitrite. The chromatographic separation was performed using BEH C-18 column and a micellar mobile phase consisted of sodium dodecyl sulphate and acetonitrile in ratio 30:70 was used. The elution of nitrite anion was accomplished in less than 1 min. Under the optimal analysis conditions, the linearity of the developed method was checked in the concentration range of 0.5-20 mg kg -1 NO 2 - with an excellent correlation coefficient of 0.996. The precisions of the method with relative standard deviation <2% was observed when standard at concentration of 1 mg kg -1 was used. The limit of detection and limit of quantitation of the developed mass spectrometric method was found to be 0.114 and 0.346 mg kg -1 , respectively. The developed UPLC/MS method was applied to quantify this anion in processed meats and poultries from various super market of Saudi Arabia (Riyadh region). The recoveries of the nitrite in the various samples were found in the range of 100.03-103.5%., Competing Interests: Compliance with ethical standardsThe authors declare that they have no conflict of interest.

Enantio-selective molecular dynamics of (±)-o,p-DDT uptake and degradation in water-sediment system is described. Both uptake and degradation processes of (-)-o,p-DDT were slightly higher than (+)-o,p-DDT enantiomer. The optimized parameters for uptake were 7.0μgL -1 concentration of o,p-DDT, 60min contact time, 5.0pH, 6.0gL -1 amount of reverine sediment and 25°C temperature. The maximum degradation of both (-)- and (+)-o,p-DDT was obtained with 16 days, 0.4μgL -1 concentration of o,p-DDT, pH 7 and 35°C temperature. Both uptake and degraded process followed first order rate reaction. Thermodynamic parameters indicated exothermic nature of uptake and degradation processes. Both uptake and degradation were slightly higher for (-)-enantiomer in comparison to (+)-enantiomer of o,p-DDT. It was concluded that both uptake and degradation processes are responsible for the removal of o,p-DDT from nature but uptake plays a crucial role. The percentage degradations of (-)- and (+)-o,p-DDT were 30.1 and 29.5, respectively. This study may be useful to manage o,p-DDT contamination of our earth's ecosystem., (Copyright © 2017. Published by Elsevier Inc.)

Magnetic nanoparticles are used in adsorptive removal of heavy metals from polluted wastewater. However, their poor stability in an acidic medium necessitates their protection with a coating layer. Coating magnetic nanoparticles with carbon showed proper protection but the heavy metal removal efficiency was slightly weak. However, to boost the removal efficiencies of surface functionalization, polyacrylamide was applied to carbon-coated Fe₃O₄ nanoparticles. In this paper, to facilitate the synthesis process, one-step carbon coating and polyacrylamide functionalization were conducted using the hydrothermal technique with the aim of enhancing the adsorptive removal capacity of Fe₃O₄ nanoparticles towards some heavy metals such as Cu(II), Ni(II), Co(II), and Cd(II). The results showed that the one-step process succeeded in developing a carbon coating layer and polyacrylamide functionality on Fe₃O₄ nanoparticles. The stability of the magnetic Fe₃O₄ nanoparticles as an adsorbent in an acidic medium was improved due to its resistance to the dissolution that was gained during carbon coating and surface functionalization with polyacrylamide. The adsorptive removal process was investigated in relation to various parameters such as pH, time of contact, metal ion concentrations, adsorbent dose, and temperature. The polyacrylamide functionalized Fe₃O₄ showed an improvement in the adsorption capacity as compared with the unfunctionalized one. The conditions for superior adsorption were obtained at pH 6; time of contact, 90 min; metal solution concentration, 200 mg/L; adsorbent dose, 0.3 g/L. The modeling of the adsorption data was found to be consistent with the pseudo-second-order kinetic model, which suggests a fast adsorption process. However, the equilibrium data modeling was consistent with both the Langmuir and Freundlich isotherms. Furthermore, the thermodynamic parameters of the adsorptive removal process, including Δ G °, Δ H °, and Δ S °, indicated a spontaneous and endothermic sorption process. The developed adsorbent can be utilized further for industrial-based applications., Competing Interests: The authors declare no conflict of interest.

The combination of magnetic nanoparticles and metal-organic frameworks (MOFs) has demonstrated their prospective for pollutant sequestration. In this work, a magnetic metal-organic framework nanocomposite (Fe 3 O 4 @AMCA-MIL53(Al) was prepared and used for the removal of U(VI) and Th(IV) metal ions from aqueous environment. Fe 3 O 4 @AMCA-MIL53(Al) nanocomposite was characterized by TGA, FTIR, SEM-EDX, XRD, HRTEM, BET, VSM (vibrating sample magnetometry), and XPS analyses. A batch technique was applied for the removal of the aforesaid metal ions using Fe 3 O 4 @AMCA-MIL53(Al) at different operating parameters. The isotherm and kinetic data were accurately described by the Langmuir and pseudo-second-order models. The adsorption capacity was calculated to be 227.3 and 285.7 mg/g for U(VI) and Th(IV), respectively, by fitting the equilibrium data to the Langmuir model. The kinetic studies demonstrated that the equilibrium time was 90 min for each metal ion. Various thermodynamic parameters were evaluated which indicated the endothermic and spontaneous nature of adsorption. The collected outcomes showed that Fe 3 O 4 @AMCA-MIL53(Al) was a good material for the exclusion of these metal ions from aqueous medium. The adsorbed metals were easily recovered by desorption in 0.01 M HCl. The excellent adsorption capacity and the response to the magnetic field made this novel material an auspicious candidate for environmental remediation technologies.

The conversion of raw biomass into C5-sugars and furfural was demonstrated with the one-pot method using Brønsted acidic ionic liquids (BAILs) without any mineral acids or metal halides. Various BAILs were synthesized and characterized using NMR, FT-IR, TGA, and CHNS microanalysis and were used as the catalyst for raw biomass conversion. The remarkably high yield (i.e. 88%) of C5 sugars from bagasse can be obtained using 1-methyl-3(3-sulfopropyl)-imidazolium hydrogen sulfate ([C 3 SO 3 HMIM][HSO 4 ]) BAIL catalyst in a water medium. Similarly, the [C 3 SO 3 HMIM][HSO 4 ] BAIL also converts the bagasse into furfural with very high yield (73%) in one-pot method using a water/toluene biphasic solvent system.

The enzyme-mimicking activity of iron oxide based nanostructures has provided a significant advantage in developing advanced molecular sensors for biomedical and environmental applications. Herein, we introduce the horseradish peroxidase (HRP)-like activity of gold-loaded nanoporous ferric oxide nanocubes (Au-NPFe 2 O 3 NC) for the development of a molecular sensor with enhanced electrocatalytic and colorimetric (naked eye) detection of autoantibodies. The results showed that Au-NPFe 2 O 3 NC exhibits enhanced peroxidase-like activity toward the catalytic oxidation of 3,3',5,5'-tertamethylbenzidine (TMB) in the presence of H 2 O 2 at room temperature (25 °C) and follows the typical Michaelis-Menten kinetics. The autoantibody sensor based on this intrinsic property of Au-NPFe 2 O 3 NC resulted in excellent detection sensitivity [limit of detection (LOD) = 0.08 U/mL] and reproducibility [percent relative standard deviation (% RSD) = <5% for n = 3] for analyzing p53-specific autoantibodies using electrochemical and colorimetric (naked eye) readouts. The clinical applicability of the sensor has been tested in detecting p53-specific autoantibody in plasma obtained from patients with epithelial ovarian cancer high-grade serous subtype (EOCHGS, number of samples = 2) and controls (benign, number of samples = 2). As Au-NPFe 2 O 3 NC possess high peroxidase-like activity for the oxidation of TMB in the presence of H 2 O 2 [TMB is a common chromogenic substrate for HRP in enzyme-linked immunosorbent assays (ELISAs)], we envisage that our assay could find a wide range of application in developing ELISA-based sensing approaches in the fields of medicine (i.e., detection of other biomarkers the same as p53 autoantibody), biotechnology, and environmental sciences.

Chemotherapy of bladder cancer has limited efficacy because of the short retention time of drugs in the bladder during therapy. In this research, nanoparticles (NPs) with a new core/shell/corona nanostructure have been synthesized, consisting of iron oxide (Fe 3 O 4 ) as the core to providing magnetic properties, drug (doxorubicin) loaded calcium phosphate (CaP) as the shell for pH-responsive release, and arginylglycylaspartic acid (RGD)-containing peptide functionalized alginate as the corona for cell targeting (with the composite denoted as RGD-Fe 3 O 4 /CaP/Alg NPs). We have optimized the reaction conditions to obtain RGD-Fe 3 O 4 /CaP/Alg NPs with high biocompatibility and suitable particle size, surface functionality, and drug loading/release behavior. The results indicate that the RGD-Fe 3 O 4 /CaP/Alg NPs exhibit enhanced chemotherapy efficacy toward T24 bladder cancer cells, owing to successful magnetic guidance, pH-responsive release, and improved cellular uptake, which give these NPs great potential as therapeutic agents for future in vivo drug delivery systems.

Highly ordered mesoporous resol-type phenolic resin and the corresponding mesoporous carbon materials were synthesized by using poly(ethylene oxide-b-caprolactone) (PEO-b-PCL) diblock copolymer as a soft template. The self-assembled mesoporous phenolic resin was found to form only in a specific resol concentration range of 40-70 wt % due to an intriguing balance of hydrogen-bonding interactions in the resol/PEO-b-PCL mixtures. Furthermore, morphological transitions of the mesostructures from disordered to gyroid to cylindrical and finally to disordered micelle structure were observed with increasing resol concentration. By calcination under nitrogen atmosphere at 800 °C, the bicontinuous mesostructured gyroid phenolic resin could be converted to mesoporous carbon with large pore size without collapse of the original mesostructure. Furthermore, post-treatment of the mesoporous gyroid phenolic resin with melamine gave rise to N-doped mesoporous carbon with unique electronic properties for realizing high CO 2 adsorption capacity (6.72 mmol g -1 at 0 °C)., (© 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Iron pyrite has long been an attractive material for environmental and energy applications, but is hampered by a lack of control over morphology and purity. Hollow porous iron pyrite nanoparticles were synthesized by a direct sulfurization of iron oxide derived from Prussian blue. The high efficiencies of these hollow porous iron pyrite nanoparticles as effective dye-sensitized solar cell counter electrodes were demonstrated, with an efficiency of 7.31 %., (© 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.)

With the aim of a reliable biosensing exhibiting enhanced sensitivity and selectivity, this study demonstrates a dopamine (DA) sensor composed of conductive poly(3,4-ethylenedioxythiophene) nanotubes (PEDOT NTs) conformally coated with porphyrin-based metal-organic framework nanocrystals (MOF-525). The MOF-525 serves as an electrocatalytic surface, while the PEDOT NTs act as a charge collector to rapidly transport the electron from MOF nanocrystals. Bundles of these particles form a conductive interpenetrating network film that together: (i) improves charge transport pathways between the MOF-525 regions and (ii) increases the electrochemical active sites of the film. The electrocatalytic response is measured by cyclic voltammetry and differential pulse voltammetry techniques, where the linear concentration range of DA detection is estimated to be 2 × 10 -6 -270 × 10 -6 m and the detection limit is estimated to be 0.04 × 10 -6 m with high selectivity toward DA. Additionally, a real-time determination of DA released from living rat pheochromocytoma cells is realized. The combination of MOF5-25 and PEDOT NTs creates a new generation of porous electrodes for highly efficient electrochemical biosensing.

We previously succeeded to prepare stable mesoporous Cu films on Au-coated conductive working electrodes by using polystyrene-b-poly(oxyethylene) (PS 63 000 -b-PEO 26 000 ) micelles as template and sulfuric acid to increase ionic conductivity. In the present study, we report the preparation of mesoporous Cu films on Cu foil. By changing the Cu salts and electrodeposition potentials, we discuss how these parameters influence the final product. Without having to filtrate interefering species, such as uric acid, ascorbic acid and glucose, the dopamine concentration can be precisely determined by applying a suitable potential. Therefore, non-invasive electrochemical sensing based on mesoporous films will be useful for daily diagnosis of mental disorder., (© 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.)

A substantive approach converting waste date pits to mercerized mesoporous date pit activated carbon (DPAC) and utilizing it in the removal of Cd(II), Cu(II), Pb(II), and Zn(II) was reported. In general, rapid heavy metals adsorption kinetics for Co range: 25-100 mg/L was observed, accomplishing 77-97% adsorption within 15 min, finally, attaining equilibrium in 360 min. Linear and non-linear isotherm studies revealed Langmuir model applicability for Cd(II) and Pb(II) adsorption, while Freundlich model was fitted to Zn(II) and Cu(II) adsorption. Maximum monolayer adsorption capacities (qm) for Cd(II), Pb(II), Cu(II), and Zn(II) obtained by non-linear isotherm model at 298 K were 212.1, 133.5, 194.4, and 111 mg/g, respectively. Kinetics modeling parameters showed the applicability of pseudo-second-order model. The activation energy (Ea) magnitude revealed physical nature of adsorption. Maximum elution of Cu(II) (81.6%), Zn(II) (70.1%), Pb(II) (96%), and Cd(II) (78.2%) were observed with 0.1 M HCl. Thermogravimetric analysis of DPAC showed a total weight loss (in two-stages) of 28.3%. Infra-red spectral analysis showed the presence of carboxyl and hydroxyl groups over DPAC surface. The peaks at 820, 825, 845 and 885 cm-1 attributed to Zn-O, Pb-O, Cd-O, and Cu-O appeared on heavy metals saturated DPAC, confirmed their binding on DPAC during the adsorption.

In this study, the determination of noxious heavy metals, cadmium (Cd), bismuth (Bi), mercury (Hg), titanium (Ti), lead (Pb) and metalloid arsenic (As) in skin-whitening cosmetics were examined using microwave digestion and inductively coupled plasma atomic emission spectrometry method. A complete digestion of cosmetics samples was achieved using a mixture of hydrofluoric acid/hydrogen peroxide/nitric acid. The quantification of the target compounds was done by standard addition method. The excellent quality parameters for instance, detection limits, As (4.6 ppb), Bi (7.9 ppb), Cd (0.45 ppb), Hg (3.3 ppb), Pb (3.8 ppb), Ti (4.3 ppb), linearity ( r 2  > 0.999) and run-to-run and day-to-day precisions with relative standard deviations <3% were obtained. The recovery rates for standard reference materials were found between 90 and 105%. The average concentration of heavy metals in cosmetics samples were in the range of 1.0-12.3 (μg g -1 , As), 33-7097 (μg g -1 , Bi), 0.20-0.6 (μg g -1 , Cd), 0.70-2700 (μg g -1 , Hg), 1.20-143 (μg g -1 , Pb) and 2.0-1650 (μg g -1 , Ti).

With the aim of preparing high performance oxide-dispersion-strengthened tungsten based alloys by powder metallurgy, the W-Y 2 O 3 composite nanopowder precursor was fabricated by an improved wet chemical method with anion surfactant sodium dodecyl sulfate (SDS) addition. It is found that the employment of SDS can dramatically decrease W grain size (about 40 nm) and improve the size uniformity. What's more, SDS addition can also remarkably improve the uniform dispersion of Y 2 O 3 particles during the synthesis process. For the alloy whose powder precursor was fabricated by traditional wet chemical method without SDS addition, only a few Y 2 O 3 dispersoids with size of approximate 10-50 nm distribute unevenly within tungsten grains. Nevertheless, for the sintered alloy whose powder precursor was produced by improved wet chemical method, the Y 2 O 3 dispersoids (about 2-10 nm in size) with near spherical shape are dispersed well within tungsten grains. Additionally, compared with the former, the alloy possesses smaller grain size (approximate 700 nm) and higher relative density (99.00%). And a Vickers microhardness value up to 600 Hv was also obtained for this alloy. Based on these results, the employment of SDS in traditional wet chemical method is a feasible way to fabricate high performance yttria-dispersion-strengthened tungsten based alloys.

Chiral resolution of baclofen, bupropion, and etodolac profens was obtained with amylose derivatized chiral reversed stationary phase (carbamate groups). The eluent used for bupropion and etodolac was MeOH-water (20:80, v/v) and for baclofen was water-methanol (95:5, v/v). The eluent run rates, finding wavelength and temperature, were 1.0 mL/min, 220 nm and 27 ± 1 °C for all the eluents. The magnitude of the retardation factors for S- and R-enantiomers of baclofen, bupropion, and etodolac were 1.37, 2.62, 2.25, 3.25, 1.8, and 3.0. The magnitudes of separation and resolution factors were 1.90, 1.44, and 1.67 and 2.77, 2.35, and 2.04. Limits of detection and quantitation were 1.0-2.0 and 5.1-10.0 μg/mL. Chiral recognition mechanisms were recognized by simulation and high-performance liquid chromatography (HPLC) experiments. It was seen that hydrogen interactions, hydrophobic interactions, and π-π exchanges were the chief interactions for chiral recognition mechanisms. The described methods may be exploited for the chiral separation of baclofen, bupropion, and etodolac profens in any unknown sample., (© 2017 Wiley Periodicals, Inc.)

A series of porous carbon spheres with precisely adjustable mesopores (4-16 nm), high specific surface area (SSA, ∼2000 m 2 g -1 ), and submicrometer particle size (∼300 nm) was synthesized through a facile coassembly of diblock polymer micelles with a nontoxic dopamine source and a common postactivation process. The mesopore size can be controlled by the diblock polymer, polystyrene-block-poly(ethylene oxide) (PS-b-PEO) templates, and has an almost linear dependence on the square root of the degree of polymerization of the PS blocks. These advantageous structural properties make the product a promising electrode material for electrochemical capacitors. The electrochemical capacitive performance was studied carefully by using symmetrical cells in a typical organic electrolyte of 1 M tetraethylammonium tetrafluoroborate/acetonitrile (TEA BF 4 /AN) or in an ionic liquid electrolyte of 1-ethyl-3-methylimidazolium tetrafluoroborate (EMIMBF 4 ), displaying a high specific capacitance of 111 and 170 F g -1 at 1 A g -1 , respectively. The impacts of pore size distribution on the capacitance performance were thoroughly investigated. It was revealed that large mesopores and a relatively low ratio of micropores are ideal for realizing high SSA-normalized capacitance. These results provide us with a simple and reliable way to screen future porous carbon materials for electrochemical capacitors and encourage researchers to design porous carbon with high specific surface area, large mesopores, and a moderate proportion of micropores.

Highly ordered mesostructured vanadium phosphonates (VP) have been synthesized in the presence of cetyltrimethylammonium bromide (CTAB) as a structure-directing agent. Nitrilotris(methylene)triphosphonic acid (NMPA) and (ammonium/sodium) metavanadate (NH 4 VO 3 /NaVO 3 ) have been used for the construction of pore walls. The CTAB templates are removed from the materials by an extraction process without destroying the parent mesostructure. The formation mechanism for the ordered mesoporous structure and its impact on electrochemical application in lithium ion batteries (LIBs) are explained by considering the structural and electrochemical stability of the framework. The results demonstrate that the counter cations (NH 4 + /Na + ) of the metavanadate precursors have a crucial role in stabilizing the mesoporous structure of the mesoporous VP materials. Mesoporous VP materials with highly ordered structure have great applicability as high-performance electrode materials in LIBs due to the advantages of their large contact area with electrolyte and short transport paths for lithium ions. Mesoporous VP electrodes exhibit high reversible specific capacity with superb cycling stability (100 cycles) and excellent retention of capacity (92 %)., (© 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.)

The present work describes the outcomes of the assessment on acrylamide contents in a number of thermally treated foods (Arabic coffee Qahwa, coffee and tea) obtained from the Saudi Arabian markets. A total of 56 food samples of different brands and origin were studied, the amounts of acrylamide in Arabic coffee Qahwa, coffee and tea were obtained in the range of 10 to 682 μg kg -1 . In comparison to coffee (152-682 μg kg -1 ), the Arabic coffee Qahwa (73-108 μg kg -1 ) and tea (10-97 μg kg -1 ) contain lower amounts of acrylamide. Among the analyzed samples, the green tea contained low amounts of acrylamide ranged from 10 to 18 μg kg -1 , and thus the green tea could be considered as a healthier hot drink. A great variation of acrylamide formation has been observed in these food products. This divergence may be due to the initial concentration of amino acids especially asparagines and reducing sugars in food products, in addition to roasting temperature and time, pH and water activity. The obtained data can also be used in epidemiological investigation to estimate the acrylamide exposure from nutritional survey., Competing Interests: The authors declare no competing financial interests.

To develop low-cost and efficient oxygen reduction reaction (ORR) catalysts, a novel hybrid comprising cobalt-embedded nitrogen-doped carbon nanotubes and nitrogen-doped reduced graphene oxide (Co-NCNT/NrGO-800) was simply prepared by pyrolysis. The combination of nanotubes and graphene, and the efficient doping with cobalt and nitrogen, greatly contribute to the excellent ORR performance. This optimized Co-NCNT/NrGO catalyst exhibits a positive onset potential of 0.91 V and a half-wave potential of 0.82 V, combined with a relatively low peroxide yield, better durability, and better methanol tolerance than commercially available Pt/C, which makes it a promising candidate as a low-cost and effective non-precious-metal ORR catalyst., (© 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Aim and Objective: The population of diabetic patients is rapidly increasing globally. The treatment of these patients is a complex phenomenon due to the use of the different drugs. The present article reports a synchronized fast SPE-UFLC separation of eight antidiabetic drugs in human plasma. Inexpensive solid phase extraction (SPE) and ultra fast liquid chromatography (UFLC) methods were presented for monitoring of eight antidiabetic drugs in human plasma. The separated drugs include metformin HCl, vildagliptin, gliclazide, linagliptin, sitagliptin, pioglitazone, glimepiride and repaglinide plasma sample., Material and Method: The column used was a Sunshell C18 (150 x 4.6 mm, 2.6 μ) with eluent of acetate buffer (0.05% TEA in 0.05 M NH4Ac of pH 7.0 with H 3PO4) - ACN (60 : 40, v/v). The flow rate was 1.0 mL/min with a detection wavelength of 210 nm and column temp. of 45±1ºC. These drugs were extracted from human plasma using Sep-Pac C18 cartridge. Phosphate buffer (25 mM; pH 7.0) containing these drugs were allowed to pass through cartridge at 0.1 mL/min flow rate. The adsorbed drugs on C18 cartridge were eluted by methanol at 1.0 mL/min flow rate., Results: The values for the retention, separation and resolution factors were ranged from 0.072 to 9.140, 1.443 to 4.208 and 2.147 to 18.652, correspondingly. The percent recoveries for these drugs in the standard laboratory samples prepared in water ranged from 77 to 88%. These values in plasma samples ranged from 10 to 22%., Conclusion: The validated method was fruitfully adopted to analyze these drugs in human plasma for the clinical monitoring of these drugs., (Copyright© Bentham Science Publishers; For any queries, please email at epub@benthamscience.org.)

A simple, fast, highly efficient and direct method using ultra-performance liquid chromatography coupled to mass spectrometry has been established for the simultaneous separation, identification and quantitation of a few saturated and unsaturated fatty acids in olive oils from various countries. No sample pretreatment techniques were employed such as extraction or derivatization for the analysis of target acids from oil samples, as the oil samples were just diluted, filtered and then directly injected to the instrument. The chromatographic separations of all target fatty acids were achieved on a Hypersil Gold C18 column of particle size 1.9μm, 50×2.1mm I.D, while the gradient elution using a binary mobile phase mixture of acetonitrile and water at a flow rate of 1.5ml/min was adopted for achieving optimum separations. The identification and quantitation of target compounds was accomplished using selected ion reaction monitoring mode. The recoveries of the fatty acids were obtained higher than 89% with good validation parameters; linearity (r(2)>0.992), detection limit between 0.09 and 0.24μg/ml, run to run and day to day precisions with percent relative standard deviation lower than 2.4% at both low (1μg/ml) and medium (10μg/ml) concentration levels. The total content of fatty acids in each individual oils was found in the range of 472.63-7751.20μg/ml of olive oil, while oleic acid was found to be the major fatty acid among all analyzed oils with the amount 3785.94μg/ml (maximum) in Syrian olive oil. The obtained validation parameters confirm that the proposed analytical method is rapid, sensitive, reproducible and simple and it could be applied for the successful evaluation of fatty acids in various oils and other matrices. All the fatty acids were efficiently eluted in a time of less than 8min with well resolved peaks by employing the proposed method., (Copyright © 2016 Elsevier B.V. All rights reserved.)

N-Acetylcysteine (NAC) is the N-acetyl derivative of the amino acid l-cysteine and is extensively used as a medicine to treat a variety of diseases. High-throughput ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS) method has been developed for the quantitative assessment of N-acetyl-l-cysteine. The method was further applied to study the distribution of the intraperitoneal injected drug into different tissues and plasma of Wistar rats, including liver, kidney, heart, lungs and spleen. The drug was having highest concentration in plasma and liver followed by kidney, lungs, heart and spleen. Method validation studies suggested being linear in the range of 1-15 µg mL(-1) for liver, kidney, heart, lungs and spleen and 1-120 µg mL(-1) for the plasma. The limit of detection and limit of quantitation were found to be 0.20 and 0.66 µg mL(-1), respectively. The recovery studies suggested that in all the cases, the obtained recovery was in the range of 98.51-101.88%. Our analyses provide a validated UPLC-MS method for the determination of NAC and its successful application for the analysis in plasma and tissues obtained from Wistar rats., (© The Author 2016. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.)

Engineering the size, composition, and morphology of platinum-based nanomaterials can provide a great opportunity to improve the utilization efficiency of electrocatalysts and reinforce their electrochemical performances. Herein, three-dimensional platinum-palladium hollow nanospheres with a dendritic shell (PtPd-HNSs) are successfully fabricated through a facile and economic route, during which SiO2 microspheres act as the hard template for the globular cavity, whereas the triblock copolymer F127 contributes to the formation of the dendritic shell. In contrast with platinum hollow nanospheres (Pt-HNSs) and commercial platinum on carbon (Pt/C) catalyst, the novel architecture shows a remarkable activity and durability toward the methanol oxidation reaction (MOR) owing to the coupled merits of bimetallic nanodendrites and a hollow interior. As a proof of concept, this strategy is also extended to trimetallic gold-palladium-platinum hollow nanospheres (AuPdPt-HNSs), which paves the way towards the controlled synthesis of other bi- or multimetallic platinum-based hollow electrocatalysts., (© 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Interference of organic compounds in the matrix of heavy metal solution could suppress their pre-concentration and detection processes. Therefore, this work aimed to develop simple and facile methods for separation of heavy metals before ICP-MS analysis. Fe3O4@SiO2@TiO2 core-double shell magnetic adsorbent was prepared and characterized by TEM, SEM, FTIR, XRD and surface area, and tested for Magnetic Solid Phase Extraction (MSPE) of Cu(II), Zn(II), Cd(II) and Pb(II). TEM micrograph of Fe3O4@SiO2@TiO2 reveals the uniform coating of TiO2 layer of about 20nm onto the Fe3O4@SiO2 nanoparticles and indicates that all nanoparticles are monodispersed and uniform. The saturation magnetization from the room-temperature hysteresis loops of Fe3O4 and Fe3O4@SiO2@TiO2 was found to be 72 and 40emug(-1), respectively, suggesting good separability of the nanoparticles. The Fe3O4@SiO2@TiO2 showed maximum adsorption capacity of 125, 137, 148 and 160mgg(-1) for Cu(II), Zn(II), Cd(II) and Pb(II) respectively, and the process was found to fit with the second order kinetic model and Langmuir isotherm. Fe3O4@SiO2@TiO2 showed efficient photocatalytic decomposition for tartrazine and sunset yellow (consider as Interfering organic compounds) in aqueous solution under the irradiation of UV light. The maximum recovery% was achieved at pH 5, by elution with 10mL of 2M nitric acid solution. The LODs were found to be 0.066, 0.049, 0.041 and 0.082µgL(-1) for Cu(II), Zn(II), Cd(II) and Pb(II), respectively while the LOQs were found to be 0.20, 0.15, 0.12 and 0.25µgL(-1) for Cu(II), Zn(II), Cd(II) and Pb(II), respectively., (Copyright © 2016 Elsevier B.V. All rights reserved.)

The effect of mechanical stirring on sol-gel synthesis of thorn-like ZnO nanoparticles (ZnO-NPs) and antimicrobial activities is successfully reported in this study. The in-house synthesized nanoparticles were characterized by XRD, SEM, TEM, FTIR, TGA, DSC and UV-visible spectroscopy. The X-Ray Diffraction analysis revealed the wurtzite crystal lattice for ZnO-NPs with no impurities present. The diametric measurements of the synthesized thorn-like ZnO-NPs (morphology assessed by SEM) were well accounted to be less than 50 nm with the help of TEM. Relative decrease in aspect ratio was observed on increasing the agitation speed. The UV-visible spectroscopy showed the absorption peaks of the ZnO-NPs existed in both UVA and UVB region. A hypsochromic shift in λmax was observed when stirring pace was increased from 500 rpm to 2000 rpm. The FTIR spectroscopy showed the absorption bands of the stretching modes of Zn-O between 500 cm(-1) to 525 cm(-1). The Thermal analysis studies revealed better stability for ZnO-NPs prepared at 2000 rpm (ZnO-2000 rpm). TGA revealed the weight loss between two main temperatures ranges viz. around (90 °C-120 °C) and (240 °C-280 °C). Finally, the effect of ZnO-NPs prepared at different stirring conditions on the growth of Gram-positive (Bacillus subtilis), Gram-negative (Escherichia coli) bacteria and a fungi (Candida albicans) were examined; which showed good antibacterial as well as antifungal properties. These findings introduce a simple, inexpensive process to synthesize ZnO-NPs using conventional methods without the use of sophisticated equipments and its application as a potent nano-antibiotic.

A rapid, sensitive and precise method for the determination of bromate (BrO3(-)), nitrate (NO3(-)) and nitrite (NO2(-)) in drinking water was developed with Ultra performance Liquid Chromatography-Mass Spectrometry (UPLC-ESI/MS). The elution of BrO3(-), NO3(-) and NO2(-) was attained in less than two minutes in a reverse phase column. Quality parameters of the method were established; run-to-run and day-to-day precisions were <3% when analysing standards at 10 µg L(-1). The limit of detection was 0.04 µg NO2(-) L(-1) and 0.03 µg L(-1) for both NO3(-)and BrO3(-). The developed UPLC-ESI/MS method was used to quantify these anions in metropolitan water from Saudi Arabia (Jeddah, Dammam and Riyadh areas) and commercial bottled water (from well or unknown source) after mere filtration steps. The quantified levels of NO3(-) were not found to pose a risk. In contrast, BrO3(-) was found above the maximum contaminant level established by the US Environmental Protection Agency in 25% and 33% of the bottled and metropolitan waters, respectively. NO2(-) was found at higher concentrations than the aforementioned limits in 70% and 92% of the bottled and metropolitan water samples, respectively. Therefore, remediation measures or improvements in the disinfection treatments are required. The concentrations of BrO3(-), NO3(-) and NO2(-) were mapped with Principal Component analysis (PCA), which differentiated metropolitan water from bottled water through the concentrations of BrO3(-) and NO3(-) mainly. Furthermore, it was possible to discriminate between well water; blend of well water and desalinated water; and desalinated water. The point or source (region) was found to not be distinctive., (Copyright © 2016. Published by Elsevier B.V.)

Certain bimetallic nanocrystals (NCs) possess promising catalytic properties for electrochemical energy conversion. Herein, we report a facile method for the one-step synthesis of porous dendritic PtNi NCs in aqueous solution at room temperature that contrasts with the traditional multistep thermal decomposition approach. The dendritic PtNi NCs assembled by interconnected arms are efficient catalysts for the oxygen reduction reaction. This direct and efficient method is favorable for the up-scaled synthesis of active catalysts used in electrochemical applications., (© 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

Unlabelled: Thermodynamic characterization of butyl methacrylate-co-ethylene dimethacrylate neat monolith and zeolitic imidazolate framework-8 incorporated with butyl methacrylate-co-ethylene dimethacrylate composite monolith were studied using inverse gas chromatography at infinite dilution under 1MPa column pressure and various column temperatures. The free energy of adsorption (ΔGA), enthalpy of adsorption (ΔHA) and entropy of adsorption (ΔSA) were determined using a series of n-alkanes. The dispersive component of surface energy (γS(D)) was estimated by Dorris-Gray and Schultz et al., Methods: The composite monolith showed a more energetic surface than the neat monolith. The acidic, KA, and basic, KD, parameters for both materials were estimated using a group of polar probes. A basic character was concluded with more basic behavior for the neat monolith. Flory-Huggins parameter, χ, was taken as a measure of miscibility between the probes with the low molecular weight and the high molecular weight monolith. Inverse gas chromatography provides a better understanding of the role of incorporated zeolitic imidazolate framework (ZIF-8) into the polymer matrix in its monolithic form., (Copyright © 2016 Elsevier B.V. All rights reserved.)

Natural products from wild and medicinal plants, either in the form of crude extracts or pure compounds provide unlimited opportunities for new drug leads owing to the unmatched availability of chemical diversity. In the present study, the cytotoxic potential of crude ethanolic extract of Ochradenus arabicus was analyzed by MTT cell viability assay in MCF-7 adenocarcinoma breast cancer cells. We further investigated its effect against oxidative stress induced by anticancer drug doxorubicin. In addition, Ultra Performance Liquid Chromatography-Mass Spectrometry (UPLC-MS) based chromatographic profiling of crude extract of O. arabicus was performed. The MTT assay data showed that the extract is moderately toxic to the MCF-7 cells. However, its treatment alone does not induce oxidative stress while doxorubicin increases the level of oxidative stress in MCF-7 cells. Whereas, simultaneous treatment of plant extract and doxorubicin significantly (p < 0.05) decreased the level of intracellular reactive oxygen species (ROS) and lipid peroxidation while an increase in the reduced glutathione and superoxide dismutase activity was observed in time and dose dependent manner. Hence, our finding confirmed cytotoxic and antioxidant potential of crude extract of O. arabicus in MCF-7 cells. However, further investigations on O. arabicus as a potential chemotherapeutic agent are needed. The analysis of bioactive compounds present in the plant extracts involving the applications of common phytochemical screening assays such as chromatographic techniques is discussed.

A monolithic capillary column containing a composite of metal-organic framework MIL-53(Al) incorporated into hexyl methacrylate-co-ethylene dimethacrylate was prepared to enhance the separation of mixtures of small aromatic compounds by using capillary liquid chromatography. The addition of 10 mg/mL MIL-53(Al) microparticles increased the micropore content in the monolithic matrix and increased the Brunauer-Emmett-Teller surface area from 26.92 to 85.12 m(2) /g. The presence of 1,4-benzenedicarboxylate moieties within the structure of MIL-53(Al) as an organic linker greatly influenced the separation of aromatic mixtures through π-π interactions. High-resolution separation was obtained for a series of alkylbenzenes (with resolution factors in the range 0.96-1.75) in less than 8 min, with 14 710 plates/m efficiency for propylbenzene, using a binary polar mobile phase of water/acetonitrile in isocratic mode. A reversed-phase separation mechanism was indicated by the increased retention factor and resolution as the water percentage in the mobile phase increased. A stability study on the composite column showed excellent mechanical stability under various conditions. The higher resolution and faster separation observed at increased temperature indicated an exothermic separation, whereas the negative values for the free energy change of transfer indicated a spontaneous process., (© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

With the evolution of nanoscience and nanotechnology, studies have been focused on manipulating nanoparticle properties through the control of their size, composition, and morphology. As nanomaterial research has progressed, the foremost focus has gradually shifted from synthesis, morphology control, and characterization of properties to the investigation of function and the utility of integrating these materials and chemical sciences with the physical, biological, and medical fields, which therefore necessitates the development of novel materials that are capable of performing multiple tasks and functions. The construction of multifunctional nanomaterials that integrate two or more functions into a single geometry has been achieved through the surface-coating technique, which created a new class of substances designated as core-shell nanoparticles. Core-shell materials have growing and expanding applications due to the multifunctionality that is achieved through the formation of multiple shells as well as the manipulation of core/shell materials. Moreover, core removal from core-shell-based structures offers excellent opportunities to construct multifunctional hollow core architectures that possess huge storage capacities, low densities, and tunable optical properties. Furthermore, the fabrication of nanomaterials that have the combined properties of a core-shell structure with that of a hollow one has resulted in the creation of a new and important class of substances, known as the rattle core-shell nanoparticles, or nanorattles. The design strategies of these new multifunctional nanostructures (core-shell, hollow core, and nanorattle) are discussed in the first part of this review. In the second part, different synthesis and fabrication approaches for multifunctional core-shell, hollow core-shell and rattle core-shell architectures are highlighted. Finally, in the last part of the article, the versatile and diverse applications of these nanoarchitectures in catalysis, energy storage, sensing, and biomedicine are presented.

The newly developed acute kidney injury biomarkers are very important for the early and timely detection of kidney diseases. This review contains details of the analyses of several acute kidney injury biomarkers using ultra-high performance liquid chromatography-mass spectrometry in urine and plasma samples. In this review we attempt to discuss some aspects of the types of the biomarkers, patents, sample preparation, and the analyses. Besides, efforts were also made to discuss the possible uses of superficially porous (core-shell) columns in traditional and inexpensive high-performance liquid chromatography instruments. Additionally, the challenges and the future prospects are also highlighted. The present review will be useful for the academicians, scientists, and clinicians for the early detection of acute kidney injury biomarkers., (© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

A sensitive and selective ultra performance liquid chromatography-mass spectrometric method has been developed for the quantitative analysis of nitrate in meat samples. Selected ion reaction (SIR) mode was adopted to identify and quantify the nitrate. Chromatographic analyses were performed on a BEH C-18 column with a mobile phase consisting of a surfactant (Cetylpyridinium chloride) and acetonitrile in equal ratio (50/50, v/v) at a flow rate of 0.4 mL min(-1). The limit of detection and limit of quantitation of the developed method was found to be 0.0599 and 0.1817 mg kg(-1), respectively. The linearity of the proposed method was checked in the concentration range of 0.5-10 mg kg(-1) with an excellent correlation coefficient (r) of 0.997. The recovery of the nitrate in the meat samples were in the range of 98.02-98.99%., (Copyright © 2015 Elsevier B.V. All rights reserved.)

Here we report functionalized multiwalled carbon nanotubes (f-MWCNTs)-CdSe nanocrystals (NCs) as photosensitizer in photoelectrochemical cells, where f-MWCNTs were uniformly coated with CdSe NCs onto SnO2 upright standing nanosheets by using a simple electrodeposition method. The resultant blended photoanodes demonstrate extraordinary electrochemical properties including higher Stern-Volmer constant, higher absorbance, and positive quenching, etc., caused by more accessibility of CdSe NCs compared with pristine SnO2-CdSe photoanode. Atomic and weight percent changes of carbon with f-MWCNTs blending concentrations were confirmed from the energy dispersive X-ray analysis. The morphology images show a uniform coverage of CdSe NCs over f-MWCNTs forming a core-shell type structure as a blend. Compared to pristine CdSe, photoanode with f-MWCNTs demonstrated a 257% increase in overall power conversion efficiency. Obtained results were corroborated by the electrochemical impedance analysis. Higher scattering, more accessibility, and hierarchical structure of SnO2-f-MWCNTs-blend-CdSe NCs photoanode is responsible for higher (a) electron mobility (6.89 × 10(-4) to 10.89 × 10(-4) cm(2) V(-1) S(1-)), (b) diffusion length (27 × 10(-6)),, ((c) average electron lifetime (32.2 ms), and transit time (1.15 ms).)

Metal-semiconductor (MS) junction between Mo and CdTe, which is one of the fundamental issues for CdTe based solar cell, has been investigated for films deposited on different substrates. XRD pattern of Mo/CdTe films on the polyimide (PI) substrate shows a strong preferential orientation of MoTe2 in (100) at 2θ = 29.44 degrees, which becomes less apparent as deposition time of CdTe increases. However, on soda lime glass (SLG) no such XRD reflection pattern is observed. Moreover, from EDX measurement, Mo-Te compound also identifies MoTe2 at Mo/CdTe interface on PI substrate, which is not present on SLG. Bulk carrier concentration of Mo/CdTe films on PI substrate for lower deposition time of CdTe is found 1.42 x 10(18) cm(-3), which is almost equal to MoTe2. Thereafter, it decreases as CdTe growth time increases. The type of unintentionally formed MoTe2 on PI substrate is found to be n-type in nature. Lattice constants of a = 6.5 Å for CdTe and a = 3.52 Å for MoTe2 are found from nanostructure study by TEM.

Non-hydrogenated amorphous Silicon-Germanium (a-SiGe) thin films were deposited at two different base pressures by RF magnetron co-sputtering. Moreover, an ex-situ thermal annealing was carried out to investigate the material properties to be suitable as the bottom cell of multi-junction solar cells. Compositional study of the films using EDX showed Ge-rich thin films with 75 atomic% of Ge. XRD reflection study implied that all samples were entirely amorphous in nature. However, a significant improvement of morphology possibly due to low base pressure was observed while thermal annealing caused peening and reduction of surface inhomogeneity in both as-sputtered films. UV-VIS-IR analysis confirmed the FESEM results. The highest transmittance was observed in the as-deposited sample grown at 4 x 10(-5) Torr, which however reduced after thermal annealing. Tauc's model was implied for band gap determination and band gap energy as low as 1.07 eV was found in the annealed sample grown at lower base pressure (4 x 10(-6) Torr). Electrical properties of films were investigated by Hall effect measurement system and results found the reduction of resistivity with the same trend of optical band gap energy.

Activated carbon was prepared from date pits via chemical activation with H3PO4. The effects of activating agent concentration and activation temperature on the yield and surface area were studied. The optimal activated carbon was prepared at 450 °C using 55 % H3PO4. The prepared activated carbon was characterized by Fourier transform infrared spectroscopy, scanning electron microscopy, thermogravimetric-differential thermal analysis, and Brunauer, Emmett, and Teller (BET) surface area. The prepared date pit-based activated carbon (DAC) was used for the removal of bromate (BrO3 (-)). The concentration of BrO3 (-) was determined by ultra-performance liquid chromatography-mass tandem spectrometry (UPLC-MS/MS). The experimental equilibrium data for BrO3 (-) adsorption onto DAC was well fitted to the Langmuir isotherm model and showed maximum monolayer adsorption capacity of 25.64 mg g(-1). The adsorption kinetics of BrO3 (-) adsorption was very well represented by the pseudo-first-order equation. The analytical application of DAC for the analysis of real water samples was studied with very promising results.

Silver nanoparticles have been synthesized and were utilized for the enhanced luminometric estimation of moxifloxacin antibiotic. During the experimental procedure, it was clearly found that the addition of silver nanoparticles intensifies the weak chemiluminescence signal intensity of calcein-KMnO4 system by several folds. It was also obvious that the intensity enhancement was linearly proportional to the moxifloxacin concentration and this phenomenon was further utilized for the quantitative determination of target analyte. Effects of the different chemical variables during the experiment were studied to achieve best chemiluminescence signal. Under the optimized experimental parameters, the linear calibration graph was established over the moxifloxacin concentration range of 6.0 × 10(-8) M to 2.5 × 10(-6) M with coefficient of correlation (r (2)) value 0.9998. The lower detection limit was found to be 5.6 × 10(-9) M. The percentage relative standard deviation calculated from five replicate chemiluminescence measurements was found to be 2.63 %. The developed chemiluminescence technique was successfully applied to the determination of moxifloxacin in tablet formulation and spiked human urine sample.

A composite zeolitic imidazolate framework-8 (ZIF-8) with a butyl methacrylate-co-ethylene dimethacrylate (BuMA-co-EDMA) monolithic capillary column (33.5cm long×250μm i.d.) was fabricated to enhance the separation efficiency of methacrylate monoliths toward small molecules using conventional low-pressure gas chromatography in comparison with a neat butyl methacrylate-co-ethylene dimethacrylate (BuMA-co-EDMA) monolithic capillary column (33.5cm long×250μm i.d.). The addition of 10mgmL(-1) ZIF-8 micro-particles increased the BET surface area of BuMA-co-EDMA by 3.4-fold. A fast separation of five linear alkanes in 36s with high resolution (Rs≥1.3) was performed using temperature program. Isothermal separation of the same sample also showed a high efficiency (3315platesm(-1) for octane) at 0.89min. Moreover, the column was able to separate skeletal isomers, such as iso-octane/octane and 2-methyl octane/nonane. In addition, an iso-butane/iso-butylene gas mixture was separated at ambient temperature. Comparison with an open tubular TR-5MS column (30m long×250μm i.d.) revealed the superiority of the composite column in separating the five-membered linear alkane mixture with 4-5 times increase in efficiency and a total separation time of 0.89min instead of 4.67min. A paint thinner sample was fully separated using the composite column in 2.43min with a good resolution (Rs≥0.89). The perfect combination between the polymeric monolith, with its high permeability, and ZIF-8, with its high surface area and flexible 0.34nm pore openings, led to the fast separation of small molecules with high efficiency and opened a new horizon in GC applications., (Copyright © 2015 Elsevier B.V. All rights reserved.)

Chiral resolution of dl-alanine-dl-tyrosine and dl-leucine-dl-phenylalanine dipeptides was achieved on AmyCoat-RP column. The mobile phase used for dl-alanine-dl-tyrosine was acetonitrile-ammonium acetate (10mM, pH 6.0) [50:50, v/v]. It was acetonitrile-methanol-ammonium acetate (10mM; pH adjusted to 4.5 with glacial acetic acid) [50:20:30, v/v] for dl-leucine-dl-phenylalanine. The flow rate of the mobile phases was 0.8mL/min with UV detection at 275nm. The values of retention factors for ll-, dd-, dl- and ld-stereomers of dl-alanine-dl-tyrosine were 1.71, 2.86, 5.43 and 9.42, respectively. The values of separation and resolution factors were 1.67, 1.90 and 1.73 and 2.88, 6.43 and 7.90, respectively. Similarly, these values for dl-leucine-dl-phenylalanine stereomers were 1.50, 2.88, 3.50 and 4.07 (retention factors), 1.92, 1.22 and 1.62 (separation factors) and 2.67, 1.55 and 2.30 (resolution factors). The limits of detections and quantitation were ranged from 2.03 to 6.40 and 6.79 to 21.30μg/mL, respectively. The modeling studies were in agreement with the elution orders. The mechanism of chiral recognition was established by modeling and chromatographic studies. It was observed that hydrogen bondings and π-π interactions are the major forces for chiral separation., (Copyright © 2015 Elsevier B.V. All rights reserved.)

An ultra high performance liquid chromatography with mass spectrometry method has been developed for the simultaneous separation, identification and determination of 22 phenolic constituents in honey from various floral sources from Yemen. Solid-phase extraction was used for extraction of the target phenolic constituents from honey samples, while multiwalled carbon nanotubes were used as solid-phase adsorbent. The chromatographic separation of all phenolic constituents was performed on a BEH C18 column using a linear gradient elution with a binary mobile phase mixture of aqueous 0.1% formic acid and methanol. The quantitation was carried out in selected ion reaction monitoring acquisition mode. The total amount of phenolic acids, flavonoids and other phenols in each analyzed honey was found in the range of 338-3312, 122-5482 and 2.4-1342 μg/100 g of honey, respectively. 4-Hydroxybenzoic acid was found to be the major phenolic acid. The main detected flavonoid was chrysin, while cinnamic acid was found to be the major other phenol compound. The regeneration of solid phase adsorbent to be reused and recovery results confirm that the proposed method could be potentially used for the routine analysis of phenolic constituents in honey extract., (© 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.)

The chiral xenobiotics are very dangerous for all of us due to the different enantioselective toxicities of the enantiomers. Besides, these have different enantioselective bioaccumulations and behaviors in our body and other organisms. It is of urgent need to understand the enantioselective bioaccumulations, toxicities, and the health hazards of the chiral xenobiotics. The present article describes the classification, sources of contamination, distribution, enantioselective bioaccumulation, and the toxicities of the chiral xenobiotics. Besides, the efforts are also made to discuss the prevention and remedial measures of the havoc of the chiral xenobiotics. The challenges of the chiral xenobiotics have also been highlighted. Finally, future prospectives are also discussed.

Silver nanoparticles have been utilized for the enhanced chemiluminogenic estimation of fluoroquinolone antibiotic gatifloxacin. It has been found that the weak chemiluminescence intensity produced from the reaction between calcein and KMnO4 can further be strengthened by the addition of silver nanoparticles in the presence of gatifloxacin. This phenomenon has been exploited to the quantitative determination of gatifloxacin. Under the optimum experimental conditions, the calibration curves are linear over the range of 8.9×10(-9)-4.0×10(-6) M, while the limits of detections were found to be 2.6×10(-9) M with correlation coefficient value (r(2)) 0.9999. The relative standard deviation calculated from six replicate measurements (1.0×10(-4) M gatifloxacin) was 1.70%. The method was applied to pharmaceutical preparations and the results obtained were in reasonable agreement with the amount labeled on the formulations. The proposed method was also used for the determination of gatifloxacin in spiked urine samples with satisfactory results. No interference effects from some common excipients used in pharmaceutical preparations have been found., (Copyright © 2015 Elsevier B.V. All rights reserved.)

Ultra performance liquid chromatography coupled to mass spectrometry was used for the simultaneous separation and determination of reducing monosaccharides (fructose and glucose), a non-reducing disaccharide (sucrose) and oligosaccharides (kestose and nystose) in HILIC mode. The chromatographic separation of all saccharides was performed on a BEH amide column using an acetonitrile-water gradient elution. The detection was carried out using selected ion recording (SIR) acquisition mode. The validation of the proposed method showed that the limit of detection and limit of quantification values for the five analyzed compounds were in the range of 0.25-0.69μg/mL and 0.82-3.58μg/mL, respectively; while the response was linear in the range of 1-50μg/mL. The developed method showed potential usefulness for a rapid and sensitive analysis of underivatized saccharides and was used for determination of sugars in three date samples (Sefri, Mabroom, Ghassab) which were soxhlet extracted by ethanol., (Copyright © 2014 Elsevier Ltd. All rights reserved.)

The influence of Bi(3+)-doping on the magnetic and Mössbauer properties of cobalt ferrite (CoFe2O4), wherein the Fe(3+) ions are replaced by the Bi(3+) ions to form CoBixFe2-xO4 ferrites, where x = 0.0, 0.05, 0.1, 0.15 or 0.2, has been investigated. The structural and morphological properties of undoped and doped ferrites, synthesized chemically through a self-igniting sol-gel method, are initially screened using X-ray diffraction, scanning electron microscopy and Fourier transform infrared spectroscopy measurements. The changes in magnetic moment of ions, their coupling with neighboring ions and cation exchange interactions are confirmed from the Mössbauer spectroscopy analysis. The effect of Bi(3+)-doping on the magnetic properties of CoFe2O4 ferrite is examined from the vibrating sample magnetometry spectra. Saturation magnetization and coercivity values are increased initially and then decreased, as result of Bi(3+)-doping. The obtained results with improved saturation magnetization (from 26.36 to 44.96 emu g(-1)), coercivity (from 1457 to 1863 Oe) and remanence magnetization (from 14.48 to 24.63 emu g(-1)) on 0.1-0.15 mol Bi(3+)-doping of CoBixFe2-xO4 demonstrate the usefulness for magnetic recording and memory devices.

A dispersive liquid-liquid microextraction procedure for lead(II) as its 5-(4-dimethylaminobenzylidene) rhodanine complex has been established prior to its microsampling flame atomic absorption spectrometric determination. The influences of various analytical parameters including pH, solvent type and volume, dispersive solvent type and volume, 5-(4-dimethylaminobenzylidene) rhodanine amount, salt effect, and centrifugation time and speed were investigated. The effects of certain alkali, alkaline earth, and transition metal ions on the quantitative extraction of lead(II) were also studied. Quantitative recoveries were obtained at pH 6. The enrichment factor was calculated as 125. The detection limit for lead is 1.1 μg/L. The accuracy of the method was tested with the additions recovery test and analysis of the standard reference materials (SPS-WW2 waste water, NIST SRM 1515 apple leaves, and TMDA-51.3 fortified water). Applications of the present procedure were tested by analyzing water and food samples.

1-(2-Pyridylazo)-2-naphthol impregnated activated carbon cloth (PAN-imp-ACC) was prepared as a solid phase sorbent and, for the first time, was used for the simultaneous separation and preconcentration of trace amounts of lead, cadmium and nickel in water, soil and sewage sludge samples prior to determination by flame atomic absorption spectrometry (FAAS). The parameters governing the efficiency of the method were optimized, including the pH, the eluent type and volume, the sample and eluent flow rates, diverse ions effects and the sample volume. A preconcentration factor of 100 was achieved for all the metal ions, with detection limits of 0.1-2.8 µg L(-1) and relative standard deviations below 6.3%. The adsorption capacity of the PAN-imp-ACC for Pb(II), Cd(II) and Ni(II) ions was found to be 45.0 mg g(-1), 45.0 mg g(-1) and 43.2 mg g(-1), respectively. The method was validated by the analysis of the certified reference materials TMDA-64.2 fortified Lake Ontario water and BCR-146R Sewage Sludge Amended Soil (Industrial Origin). The procedure was applied to determine the analytes content in real samples., (Copyright © 2014 Elsevier Inc. All rights reserved.)