Investigation on Binding between Cations and Amides using UV Raman Spectroscopy

The interaction of proteins with salt ions plays an important role in life activities.We used butyramide as a model molecule to investigate the interaction of protein backbones with cations.The experiment was performed in an aqueous solution of metal chloride using UV Raman spectroscopy.It was found that well-hydrated metal cations(Ca^(2+),Mg^(2+))tend to bind to C=O in the amide bond,resulting in redistribution of the amide I band peaks.Specifically,the peak intensity ratio of 1655 cm^(-1)to 1610 cm^(-1)increases significantly with increasing concentrations.However,this phenomenon is not obviously observed in NaCl solution.Furthermore,we studied the effect of salt ions on the water structures.The addition of Ca^(2+)and Mg^(2+)is beneficial to the enhancement of the water signal at the 3400 cm^(-1)position,while the Na^(+)at the same concentration is not obvious.The results have shown that the interaction between cations and amides satisfies the following order:Ca^(2+)>Mg^(2+)>Na^(+),which conforms to the Hofmeister series.

Interaction between Eu-phenylalanine and DNA Using Cyclic Voltammetry and UV Spectroscopy

The interaction between DNA and the Eu(Phe) 3+ 3 complex ion has been studied by means of cyclic voltammetry and differential UV spectroscopy The results depicted an obvious decrease of peak current in CV plot after the reaction between the two species studied The observed peak potential separation was increased but the diffusion coefficient of Eu complex ion was decreased Hypochromicity was observed at 226 and 258 nm after the predicted interaction of them A preliminary interpretation is proposed for discussion

Interzeolite transformation from FAU to CHA and MFI zeolites monitored by UV Raman spectroscopy

As a powerful and sensitive tool for the characterization of zeolite building units,UV Raman spectroscopy has been used to monitor interzeolite transformation from FAU to CHA and MFI zeolites.The results show that the behavior of double 6-membered rings(D6Rs)in the FAU zeolite framework plays an important role during the formation of the target product in the interzeolite transformation.For the transformation of FAU to CHA,because both zeolites contain the same D6R units,direct transformation occurs,in which the D6Rs were largely unchanged.In contrast,for the transformation of FAU to MFI,the D6Rs can be divided into two single 6-membered rings(S6Rs),which further assembled into the MFI structure.In this crystallization,5-membered rings(5Rs)are only observed in the MFI framework formation,suggesting that the basic building units in the transformation of FAU to MFI are S6Rs rather than 5Rs.These insights will be helpful for further understanding of the interzeolite transformation.

Comparison of Nitric Oxide Concentrations in μs-and ns-Atmospheric Pressure Plasmas by UV Absorption Spectroscopy

In this paper,an absorption spectroscopy measurement method was applied on two atmospheric pressure plasma sources to determine their production of nitric oxide.The concentrations are essential for evaluating the plasma sources based on the principle of the Dielectric Barrier Discharge（DBD）for applications in plasma medicine.The described method is based on a setup with an electrodeless discharge lamp filled with a mixture of oxygen and nitrogen.One of the emitted wavelengths is an important resonance wavelength of nitric oxide（λ = 226.2 nm）.By comparing the absorption behaviour at the minimum and maximum of the spectral absorption cross section of nitric oxide around that wavelength,and measuring the change in intensity by the absorbing plasma,the concentration of nitric oxide inside the plasma can be calculated.The produced nitric oxide concentrations depend on the pulse duration and are in the range of 180 ppm to 1400 ppm,so that a distance of about 10 cm to the respiratory tract is enough to conform to the VDI Guideline 2310.

Development and validation of global prediction models for monitoring the manufacturing process of herbal medicine by ultraviolet spectroscopy

Objective: Process monitoring for traditional Chinese medicine(TCM) preparations is necessary to ensure the quality of the product. A typical pharmaceutical process of TCM preparations consists of multiple manufacturing units, such as ethanol precipitation, concentration, and water precipitation, among others. Compared with the traditional practice of one prediction model for one unit, the global model covers the variation from samples with different backgrounds or processes and can be used to monitor intermediates from substeps.Methods: We used ultraviolet(UV) spectroscopy to establish global models for a typical TCM preparation-Danhong injection.The concentrations of danshensu, protocatechualdehyde, rosmarinic acid, salvianolic acid A, salvianolic acid B, and hydroxyl safflor yellow A and the total phenolic and total sugar contents were quantified for every intermediate from operation units of Danhong injection. New samples prepared by mixing different intermediates were introduced for the calibration set to cover more variations. An accuracy profile was employed to validate the developed method from the aspects of specificity, trueness, precision,accuracy, linearity, and robustness.Results: The developed models showed a high determination coefficient(R2) value up to 0.97 and a low root-mean-square error of the prediction set. Five components of the models passed all validation tests, whereas the total sugar was not suitable for modeling with UV and did not apply to the whole process.Conclusions: This study indicates that the global models of UV spectroscopy for the quantitative determination of phenolic acids are feasible and reliable with a simple, rapid, and non-destructive method.Graphical abstract: http://links.lww.com/AHM/A22.

Analytical Method Development and Validation of Etanercept by UV and RP-UFLC Methods

The research work was carried out using Ultraviolet (UV)—visible spectroscopy and Reverse Phase-Ultra Fast Liquid Chromatography (RP-UFLC) for establishing novel methods for the analysis and quantification of Biosimilar drug, Etanercept. The maximum absorbance of Etanercept was found to be 215 nm and it obeyed Beer-Lamberts law in the range of 5 to 200 μg/ml and 1 to 32 μg/ml for UV and RP-UFLC, respectively. The correlation coefficient (r2) value was found to be between 0.999 and 0.9995. All the validation parameters like linearity, accuracy, and precision, Limit of Detection (LOD), Limit of Quantitation (LOQ) and Robustness were found to be within acceptance criteria as per ICH guidelines. The results of accuracy studies (99.0% to 100.38%) indicated the methods to be accurate. The RSD % for interday and intraday precision studies was found to be less than 2%. Robustness and ruggedness were expressed in terms of RSD % which were also in the specified limits. LOD and LOQ of proposed method was calculated and found to be 1.257 and 3.809 μg/ml by UV, and 0.1073 μg/ml and 0.3251 μg/ml by RP-UFLC method, respectively. The developed methods were observed to be simple, rapid and cost-efficient. It can be easily applied for the estimation of Etanercept in the marketed formulations and for routine analysis of the Biosimilar drug.

Analytical Method Development and Validation of Filgrastim by UV and RP-UFLC Methods

The research work was carried out for establishing a new Ultra Violet (UV)— Visible spectroscopy and Reverse phase-Ultra Fast Liquid Chromatography (RP-UFLC) method for the analysis and quantification of a biosimilar drug, Filgrastim. Filgrastim or recombinant methionyl granulocyte colony stimulating factor (rGCSF) is a glycoprotein. It has a biological action essential for proliferation and differentiation of hematopoetic and progenitor cells. The UV and RP-UFLC work was carried on a Shimadzu UV1800 Spectrophotometer and Shimadzu Prominence LC-20AD UFLC systems, respectively. The λmax of filgrastim was found to be 215 nm. The correlation coefficient by UV spectroscopy was found to be 0.9994 for the concentration range of 1 to 3 μg/ml in double distilled water. The Reverse phase UFLC was done by using Phenomenex C4 (25 cm × 0.46 cm internal diameter) 15 μ, 300 A° analytical column. The optimized mobile phase for binary elution was Acetonitrile and double distilled water (80:20) with a flow rate of 1 ml/min. The retention time of drug was at 3.2 min. It was observed that the response of the detector was linear in the range of 5 - 15 μg/ml with correlation coefficient value of 0.999. After developing the methods, it was assured for the intended use by validation of the analytical parameters like linearity, accuracy, precision, limit of detection, limit of quantitation, ruggedness and robustness. The results of all the parameters for both the methods were found to be within the acceptance criteria as per the International Council for Harmonisation (ICH) guidelines.

Propagating disturbances along a coronal loop from simultaneous EUV imaging and spectroscopic observations

Propagating disturbances（PDs） were studied along an active region loop using simultaneous imaging and spectroscopy. An image sequence recorded in the Fe Ⅸ/Fe X 171 channel, from TRACE and spectral data in the Si Ⅻ 520.6 line obtained from CDS/SOHO, are analyzed. A space-time map constructed from the TRACE image sequence shows the presence of PDs close to the loop foot point propagating with an apparent speed of 39 km s-1. The periodicity was found to be 5.4 min.The corresponding spectroscopic data from CDS, at a location away from the foot point, show oscillations in all three line parameters roughly at the same period. At locations farther from the foot point, the line width oscillation seems to disappear while the Doppler velocity oscillation becomes prominent. We attribute this to the signature of propagating slow waves that get affected by flows/other events close to the foot point. Spectral line profiles do not show much asymmetry, however, it is difficult to infer anything due to the broadened Gaussian shape of the CDS line profiles.

Direct Spectroscopic Determination of Europium（ Ⅱ ） Concentration During Europium（ Ⅲ ） Electro-Reduction in Hydrochloric Acid Medium

UV-Vis spectroscopy was used to directly determine the concentration of Eu（ Ⅱ） during electroreduction of Eu （ Ⅲ ） in hydrochloric acid medium. Electroreduction was carried out in a flow type electrolyzer with glassy carbon cathode at the constant potential of - 800 mV vs. Ag/AgCl. The effects of oxygen and concentration of hydrochloric acid on the system were investigated. For 0.01 mol· L^-1 hydrochloric acid, calibration curves for Eu （Ⅱ） absorption bands at 248 and 320 nm were constructed. Molar absorption coefficients were estimated to be 2016 and 648 L· mol^-1·cm^-1, respectively. The absorbance strongly decreased with decrease in pH of the solution, whereas concentration of chloride had only a negligible effect.

Syntheses,Crystal Structures and Complexing Properties of 1,3-Distal Calix[4]arene Schiff Bases

Novel 1,3-distal p-tert-butylcalix[4]arene Schiff bases were efficiently synthesized in three steps. At first p-tert-hutylcalix[4]arene was reacted with N-2-hydroxyethylphthalimide catalyzed by TPP/DEAD or alkylated with ω-hatoalkylphthalimide in the system of K2CO3/KI/CH3COCH3 to give 1,3-distal diphthalimidoalkyl calixarenes, which were in turn hydrazinolyzed to give diaminoalkyl calixarenes. Then with the aid of the condensation of active calixarene amines with salicylaldehyde, 2-hydroxy-l-naphthaldehyde or pyridine-2-carboxaldehyde, a series of 1,3-distal calixarene Schiff bases was prepared in satisfied yields. The single crystal structures and complexing properties of these Schiff bases for transition metal ions were studied.

Interactions of ginsenosides with DNA duplexes: A study by electrospray ionization mass spectrometry and UV absorption spectroscopy

The non-covalent complexes of duplexes DNA and 9 ginsenosides（1 aglycone and 8 glycosides） were investigated using electrospray ionization mass spectrometry（ESI-MS） in the gas phase. The results of relative binding affinities in negative ion mode revealed that several factors impact on the duplexbinding properties of ginsenosides. Glycosylations of 20（S）-protopanaxadiol ginsenosides at the position C-20 and 20（S）-protopanaxatriol classification at the position C-6 enhanced the fraction of bound DNA sharply. A rhamnose moiety shows little lower binding intensities than glucose at the same position.Ginsenosides of 20（S）-protopanaxatriol result in subtle higher binding affinities toward the duplex DNA than 20（S）-protopanaxadiol family. However, glycosylation with two sugar moieties does not show a higher binding affinity than with only one moiety. The collision-induced dissociation experimental data demonstrate the gas-phase stability and fragmentation patterns of the ginsenoside/DNA complexes are related to the glycoside number. Positive ion ESI mass spectra of the complexes were also recorded. The result of ESI-MS suggests that hydrogen bonds are the dominate interaction between ginsenosides and DNA. Similar results were obtained in solution-phase by UV spectroscopy, which exhibit a hyperchromism and blue-shift effect when DNA solution was titrated by individual ginsenoside.

Study of Preionization XeCl Excimer Laser and Ultraviolet Spectrum Characteristic

The pumped system of the XeCl excimer laser has been designed and applied to analyze UV XeC1 laser spectroscopy characteristics. Under the proportion of mixed gas of HCI：Xe：He = 0.1%： 1% ：98.9%, excimer laser light was generated by stable glow discharge process. The laser spectrum, pulse duration, and laser power properties were obtained. The result shows that this XeCI excimer laser exhibits unique spectral properties, with two peaks between 307.7 nm and 308.5 nm at high pressure with a pumped power of 1.3959 MW/cm^3. The transition relies on the strongest transitions between B-X and C-X. The maximum-intensity transition of spectroscopy is B to X energy levels. The laser parameters are as follows： minimal duration of 15.42 ns, a repetition rate from 0.5 Hz to 5 Hz, single pulse stable power of 400 m J, and beam divergence angle of 3 mrad. The laser can be used to study UV spectroscopy, laser ablation sampling and sputtered pinnate form.

Calcium chloride linked camel milk derived casein nanoparticles for the delivery of sorafenib in hepatocarcinoma cells

Sorafenib,a multikinase inhibitor used for the treatment of hepatocellular carcinoma,is limited by its low oral bioavailability.To overcome this drawback,we have developed novel camel milk casein-derived nanoparticles as a drug delivery system.Camel milk casein is not only biocompatible on oral administration but is actually a dietary protein of pharmaceutical relevance.Casein is used because of its amphiphilic nature,self-assembling property,ability to show sustained release,and capability of encapsulating both hydrophilic and hydrophobic drugs.In this study,camel milk casein nanoparticles loaded with sorafenib were developed and characterized.Characterization of casein nanoparticles was done by dynamic light scattering(DLS),zeta potential analysis,scanning light microscopy(SEM),and FTIR.The drug content in nanoparticle and drug-protein binding studies were conducted by UV spectroscopy.The cytotoxicity and cellular uptake efficiency studies were performed in HepG2 cell lines.It was observed that the cytotoxic effect of sorafenib loaded camel milk casein nanoparticles was more than free sorafenib in HepG2 cells.This work suggests camel milk casein as a suitable drug delivery molecule for sorafenib.In the future,it may also be used in enhancing the efficacy and specific distribution of other water-insoluble anticancer drugs.

Study on the Influence of Ni Modifying on Phase Transformation and Photocatalytic Activity of TiO_2

The Ni-modified TiO2 was synthesized using two methods including co-precipitation(Ni doped TiO2, Ni-TiO2) and wet impregnation(Ni loaded TiO2, Ni/TiO2). The surface and bulk crystalline phases of Ni-modified TiO2 were investigated by using X-ray diffractometry(XRD), UV Raman spectroscopy, TEM, and SEM. It is observed that Ni doping can promote the phase transition and grain size growth of TiO2. Moreover, the propagation of the rutile phase from the bulk into the surface region of TiO2 is increased when the Ni doping amount reaches up to 3%. However, in Ni/TiO2, it is found out that the surface and bulk phase transformation of TiO2 can be inhibited after impregnation of 1% of Ni on the TiO2. Compared with the co-precipitation method, Ni species may be more enriched in the surface of the Ni/TiO2 sample upon adoption of the impregnation method, and the direct contact of anatase particles of TiO2 is avoided. As a consequence, the phase transition in the surface and bulk region of TiO2 can be effectively inhibited by Ni loading. Additionally, the activity of the photocatalytic degradation of RhB on the 3Ni-TiO2-600 ℃ sample is higher than that on the 3 Ni/TiO2-600 ℃ sample. The phase junction formed between anatase and rutile in the surface region of 3Ni-TiO2-600 ℃ may the main reason for its high photocatalytic activity.

Conversion of methanol to propylene over SAPO-14:Reaction mechanism and deactivation

Methanol to olefins(MTO)reaction as an important non-oil route to produce light olefins has been industrialized,and received over 80% ethylene plus propylene selectivity.However,to achieve high single ethylene or propylene selectivity towards the fluctuated market demand is still full of challenge.Small-pore SAPO-14 molecular sieve is a rare MTO catalyst exhibiting extra-high propylene selectivity.It provides us a valuable clue for further understanding of the relationship between molecular sieve structure and MTO catalytic performance.In this work,a seconds-level sampling fixed-bed reactor was used to capture real-time product distributions,which help to achieve more selectivity data in response to very short catalytic life of SAPO-14.Changes in product distribution,especially during the low activity stage,reflect valuable information on the reaction pathway.Combined with in situ diffuse reflectance infrared Fourier-transform spectroscopy,in situ ultraviolet Raman measurements and ^(12)C/^(13)C isotopic switch experiments,a reaction pathway evolution from dual cycle to olefins-based cycle dominant was revealed.In addition,the deactivation behaviors of SAPO-14 were also investigated,which revealed that polymethylbenzenes have been the deactivated species in such a situation.This work provides helpful hints on the development of characteristic methanol to propylene(MTP)catalysts.

UV Spectroscopic Method for Optimization and Determination of Glibenclamide in Bulk,Pharmaceutical Dosage Form and its Application for In Vitro Interaction Studies

A simple,easy and cost-efficient UV spectroscopic method was developed and validated for glibenclamide,the second generation of sulfonylureas,using 0.1 N NaOH as a solvent.The proposed method is linear(R^(2)>0.999)with the range 5-25μg mL^(−1),accurate(99.60%),precise(inter and intraday variation 0.241 and 0.019%,respectively)and robust(<1%).The quantification and detection limit were 1.46 and 0.48μg mL^(−1),respectively.The validated method was applied for in vitro interaction studies of glibenclamide(GLB)with commonly prescribed quinolones(ciprofloxacin,levofloxacin,moxifloxacin,and gemifloxacin)and nonsteroidal anti-inflammatory drugs(NSAIDs)(diclofenac sodium,ibuprofen,mefenamic acid,and aspirin)using UV spectrophotometer.The in vitro interaction studies were carried out in different artificially prepared physiological buffers at 37°C for 2 h.Results showed raised level of glibenclamide when interacted with gemifloxacin(pH 7.4),levofloxacin(pH 9),ciprofloxacin(pH 4.5)and with moxifloxacin(pH 4.5,7.4 and 9).Interaction with NSAIDs results in increased%availability of glibenclamide in the presence of diclofenac sodium,ibuprofen,and mefenamic acid at pH 4.5.The anticipated method can be successfully applied for the routine analysis and also for the interaction of glibenclamide with other drugs.

Application of Generalized Standard Addition Method and Ultraviolet Spectroscopy to Quantify Electrolytic Depolymerization of Lignin

Industrial lignin waste is an important byproduct of bio-refineries and the paper industry.Depolymerization of industrial lignin could generate useful aromatic compounds.This group has focused on electrolytic decomposition of biorefinery lignin.To quantify electrolytic decomposition of the lignin in a highly caustic solution,ultraviolet(UV)spectroscopy provides a useful probe.The conversion of the neat lignin to the oxidized products achieved by the electrolytic reactor may be measured by quantifying the amount of unreacted neat lignin that remains in the effluent.Because the properties of electrolytic decomposition products are largely unknown,a useful approach to quantify decomposition of the neat lignin is to use a multivariate calibration method referred to as the generalized standard addition method(GSAM).In this approach,the electrolytic decomposition products represent a background interference and the neat lignin that remains can be quantified.This approach allows the conversion of the neat lignin to be calculated in a solution that is a complex mixture.

Selective elimination of chromophoric and fluorescent dissolved organic matter in a full-scale municipal wastewater treatment plant

Effluent organic matter（Ef OM） from municipal wastewater treatment plants potentially has a detrimental effect on both aquatic organisms and humans.This study evaluated the removal and transformation of chromophoric dissolved organic matter（CDOM） and fluorescent dissolved organic matter（FDOM） in a full-scale wastewater treatment plant under different seasons.The results showed that bio-treatment was found to be more efficient in removing bulk DOM（in term of dissolved organic carbon,DOC） than CDOM and FDOM,which was contrary to the disinfection process.CDOM and FDOM were selectively removed at various stages during the treatment.Typically,the low molecular weight fractions of CDOM and protein-like FDOM were more efficiently removed during bio-treatment process,whereas the humic-like FDOM exhibited comparable decreases in both bio-treatment and disinfection processes.Overall,the performance of the WWTP was weak in terms of CDOM and FDOM removal,resulting in enrichment of CDOM and FDOM in effluent.Moreover,the total removal of the bulk DOM（P 〈 0.05） and the protein-like FDOM（P 〈 0.05） displayed a significant seasonal variation,with higher removal efficiencies in summer,whereas removal of CDOM and the humic-like FDOM showed little differences between summer and winter.In all,the results provide useful information for understanding the fate and transformation of DOM,illustrating that sub-fractions of DOM could be selectively removed depending on treatment processes and seasonality.

Spontaneous Deposition of Uniformly Distributed Ruthenium Nanoparticles on Graphitic Carbon Nitride for Quantifying Electrochemically Accumulated H_(2)O_(2)

Highly dispersed ultrasmall ruthenium nanoparticles with a clean surface are deposited onto graphitic carbon nitride(C_(3)N_(4)-Ru)through spontaneous redox reaction between the C_(3)N_(4) sheets and Ru salt without the use of any reductant.The as-prepared C_(3)N_(4)-Ru exhibits distinct peroxidase-like activity.A nanozyme based method is successfully developed for detecting the H_(2)O_(2) generated in-situ by the two-electron oxygen reduction strategy.The C_(3)N_(4)-Ru nanozyme can realize the detection of H_(2)O_(2) with a wide linear range and a low detection limit.The testing results are also compared with the conventional modified titration method,and show greater possibility for the practical detection of H_(2)O_(2) produced via the electrochemical oxygen reduction for its higher selectivity.

Effect of nitrogen/phosphorus concentration on algal organic matter generation of the diatom Nitzschia palea:Total indicators and spectroscopic characterization

Critical algal blooms in great lakes increase the level of algal organic matters（AOMs）,significantly altering the composition of natural organic matters（NOMs） in freshwater of lake.This study examined the AOM＇s characteristics of Nitzschia palea（N.palea）,one kind of the predominant diatom and an important biomarker of water quality in the great lakes of China,to investigate the effect of AOMs on the variation of NOMs in lakes and the process of algal energy.Excitation–emission matrix fluorescence（EEM） spectroscopy,synchronous fluorescence（SF） spectroscopy and deconvolution UV–vis（D-UV） spectroscopy were utilized to characterize AOMs to study the effects of nutrient loading on the composition change of AOMs.From results,it was revealed that the phosphorus is the limiting factor for N.palea＇s growth and the generation of both total organic carbon and amino acids but the nitrogen is more important for the generation of carbohydrates and proteins.EEM spectra revealed differences in the composition of extracellular organic matter and intracellular organic matter.Regardless of the nitrogen and phosphorus concentrations,aromatic proteins and soluble microbial products were the main components,but the nitrogen concentration had a significant impact on their composition.The SF spectra were used to study the AOMs for the first time and identified that the protein-like substances were the major component of AOMs,creating as a result of aromatic group condensation.The D-UV spectra showed carboxylic acid and esters were the main functional groups in the EOMs,with –OCH_3,–SO_2NH_2,–CN,–NH_2,–O– and –COCH_3functional groups substituting into benzene rings.