Optimization Strategy for Isocratic Separation of α-Aspartame and Its Breakdown Products by Reversed Phase Liquid Chromatography

α-Aspartame (L-α-aspartyl-L-phenylalanine methyl ester) is increasingly being used in wide variety of commonly consumed food products. This structure contains ester and peptide bonds. The ester linkage may hydrolyze to produce L-α-aspartyl-L-phenylalanine or cyclohydrolyze to produce the corresponding diketopiperazine ring. This ring can open to form L-α-aspartyl-L-phenylalanine and ultimately this compound can hydrolyze to L-phenylalanine and L-aspartic acid. The pH, buffer type, concentration, the presence of water and temperature are other important factors affecting its stability. Because α-aspartame can lose its sweetness under these conditions determination of aspartame and its breakdown products is extremely important for diet foods quality. The optimum mobile phase for the chromatographic separation was found to be acetonitrile-water (20:80, ν/ν) with 5.10^?3 M hexanesulfonic acid and a pH of 2.6.     

Minimizing Side Product Formation in Alkyne Functionalization of Ruthenium Complexes by Introduction of Protecting Groups

The synthesis of alkyne functionalized bipyridine ruthenium complexes are reported. The improved synthetic approach through application of stable protecting groups prevents formation of possible side products while facilitating purification. By applying copper-catalysed azide-alkyne cycloaddition reactions (CuAAC) pyrene units with flexible alkyl linkers are introduced at the periphery of the complex, opening up various applications including surface immobilization and DNA intercalation. All complexes are characterized structurally as well as photophysically, especially regarding the influence of the introduced alkyne and triazolyl substituents on their photophysical behavior.     

Synthesis of Some Polymer‐Metal Complexes and Elucidation of their Structures

In this study, the nine coordination polymers of Fe(III), Co(II) and Ni(II) salts have been synthesized using polyacrylamide (PAA), polt(ethylene glycol) (PEG) and poly(vinyl alcohol) (PVA) and their structures were characterized by magnetic and conductivity measurements, ultraviolet‐visible (UV‐VIS), FTIR spectroscopy and thermogravimetric analysis (TGA). The structures of Fe(III) complexes in the all coordination polymers were found as tetrahedral. The structures of PAA‐Co(II) coordination polymer was determined as octahedral geometry whereas PEG‐Co(II) and PVA‐Co(II) complexes showed as tetrahedral structure. PAA‐Ni(II) and PEG‐Ni(II) complexes have octahedral geometry, whereas PVA‐Ni(II) has a square planar structure. Besides, the stress‐strain experiments of PVA‐metal coordination polymers obtained rubber‐like structure were carried out and the value of breaking‐strain of PVA‐Ni(II) complex was found to be about 17% of vulcanized natural rubber. The conductivities of the resulting polymer‐metal complexes were measured by four‐probe technique and were found in the range 10^?5?10^?6 Scm^?1. Thus, it was suggested that they can be used in the field potential application of conducting polymers. TGA results revealed that among the complexes PEG‐Fe(III) and PVA‐Fe(III) complexes have the highest thermally stable.     

Nutritional Analysis of Red-Purple and White-Fleshed Pitaya (Hylocereus) Species

Pitaya is one of the most preferred and produced tropical fruit species recently introduced to the Mediterrranean region in Turkey. Due to its nutritional fruits with high economic value, the popularity of pitaya increases steadily in Turkey as an alternative crop. No detailed nutritional analysis has been undertaken in Turkey so far on fruits of the pitaya species. In this study, we determined and compared some nutritional parameters in fruit flesh of two pitaya (dragon fruit) species (Hylocereus polyrhizus: Siyam and Hylocereus undatus: Vietnam Jaina) grown in the Adana province located in the eastern Mediterranean region in Turkey. The individual sugars, antioxidant activity, total phenolic content, phenolic compounds and volatiles were determined for the first time in Turkey on two pitaya species. The results showed that total phenol content and antioxidant capacity are notably higher in red-fleshed fruits than white-fleshed ones and the predominant phenolic compound in fruits of both species was quercetin. The total sugar content and most of the phenolic compounds in fruits of two pitaya species were similar. A total of 51 volatile compounds were detected by using two Solid Phase Micro Extraction (SPME) fibers, coupled with Gas Chromatography Mass Spectrometry (GC-MS) techniques, and more volatile compounds were presented in the white-fleshed species. Total phenolic content (TPC) of the red-fleshed and white-fleshed pitaya species were 16.66 and 17.11 mg GAE/100 g FW (fresh weight). This study provides a first look at the biochemical comparison of red-fleshed and white-fleshed pitaya species introduced and cultivated in Turkey. The results also showed, for the first time, the biochemical content and the potential health benefit of Hylocereus grown in different agroecological conditions, providing important information for pitaya researchers and application perspective.     

Examination of performance of glassy carbon paste electrode modified with gold nanoparticle and xanthine oxidase for xanthine and hypoxanthine detection

A composite electrode was prepared by modifying glassy carbon microparticles with gold nanoparticles (Au-nps) and xanthine oxidase enzyme (XOD) for xanthine (X) and hypoxanthine (Hx) detection. After the optimization of the system for X, the biosensor was characterized for X and Hx. A linearity was obtained in the concentration range between 5.00 × 10⁻⁷ and 1.00 × 10⁻⁵ M for X with equation of y = 0.24x + 0.712 and 5.00 × 10⁻⁶ to 1.50 × 10⁻⁴ M for Hx, with equation of y = 0.014x + 0.575, respectively. Obtained results were compared to X and/or Hx biosensors including/not including Au-np in the structure. The developed system was also applied for detection of Hx in canned tuna fish sample and very promising results were obtained.     

Structural and Optical Properties of Zinc Nitride Films Prepared by Pulsed Filtered Cathodic Vacuum Arc Deposition

Polycrystalline zinc nitride films are deposited on Coming 7059 glass substrates by pulsed filtered cathodic vacuum arc deposition （PFCVAD）. The crystallographic structure is studied by means of x-ray diffraction. These measurements show that all the films are crystallized in the cubic structure, in a preferred orientation along the （332） and （631） directions. Weak XRD signal shows small crystallites distributed in an amorphous tissue. A small improvement of crystallinity is observed with annealing. Optical parameters such as absorption, energy band gap, Urbach tail, extinction coefficients have been determined. The Urbach tail energy is decreased with annealing at 500℃ for one hour. Energy band gap values are found to be increased by annealing.     

Comparison of the band alignment of strained and strain-compensated GaInNAs QWs on GaAs and InP substrates

We present a comparison of the band alignment of the Ga_1−xIn_xN_yAs_1−y active layers on GaAs and InP substrates in the case of conventionally strained and strain-compensated quantum wells. Our calculated results present that the band alignment of the tensile-strained Ga_1−xIn_xN_yAs_1−y quantum wells on InP substrates is better than than that of the compressively strained Ga_1−xIn_xN_yAs_1−y quantum wells on GaAs substrates and both substrates provide deeper conduction wells. Therefore, tensile-strained Ga_1−xIn_xN_yAs_1−y quantum wells with In concentrations of x0.53 on InP substrates can be used safely from the band alignment point of view when TM polarisation is required. Our calculated results also confirm that strain compensation can be used to balance the strain in the well material and it improves especially the band alignment of dilute nitride Ga_1−xIn_xN_yAs_1−y active layers on GaAs substrates. Our calculations enlighten the intrinsic superiority of N-based lasers and offer the conventionally strained and strain-compensated Ga_1−xIn_xN_yAs_1−y laser system on GaAs and InP substrates as ideal candidates for high temperature operation.     

WDS versus silicon drift detector EDS: a case report for the comparison of quantitative chemical analyses of natural silicate minerals

Electron probe microanalysis (EPMA) is an essential analytical approach to determine elemental concentrations of various solid specimens quantitatively in mineralogical, petrological and materials research. Either wavelength dispersive X-ray (WDS) or energy dispersive X-ray (EDS) spectrometric techniques can collect the characteristic X-rays generated from each element in the specimen by an incident electron beam in order to define chemical constituents. Although WDS has been the preferred technique because of its higher spectral resolution and ability to detect trace elements, new generation EDS systems with silicon drift detectors (SDD), equipped with thin windows and integrated digital processing electronics, are claimed to approach the WDS throughput. In this study, we compared the analytical capability of a SDD EDS system with respect to WDS equipped systems on natural silicate minerals. For this purpose, natural rock samples, in which the silicate minerals present had already been analysed by various WDS systems, were chosen to compare these results with the ones acquired with a SDD EDS system. SDD EDS yielded satisfactory results for major elements (Na, Mg, Al, Si, K, Ca, Ti, Mn and Fe) compared with the results of the same minerals obtained by various WDS systems.     

Quantitative analysis of ezetimibe in human plasma by gas chromatography‐mass spectrometry

A new, specific and sensitive GC‐MS method with electron impact ionization technique was developed for quantitative analysis of ezetimibe (EZE) in human plasma. Prior to GC analysis, EZE was derivatized with N‐methyl‐N‐trimethylsilyl‐trifluoroacetamide (MSTFA), which is a trimethyl silylating reagent. The derivatization reaction was optimized and parameters such as catalyst, derivatization time, temperature, solvent and the volume of silylating reagent were investigated. Trimethylsilyl ether derivative of EZE was determined in selected ion monitoring (SIM, mass‐to‐charge ratio (m/z): 326) mode. The method was validated with respect to LOD and LOQ, precision, accuracy, linearity, specificity, stability, and recovery. The LOQ and LOD were found as 15 and 10 ng/mL, respectively. The linearity of the method ranged from 15 to 250 ng/mL. The correlation coefficient of the calibration curve was 0.9977 ± 0.0004 (± S.E.M.). The intra‐ and inter‐day precisions (RSD) were less than 6% and accuracies (bias) for intra‐ and inter‐day accuracy were found between –4.04 and 9.71% at four different concentration levels (15, 40, 100, 250 ng/mL). The proposed method was successfully applied to real human plasma samples for determination of total EZE.