2nd International Conference and Expo on Separation Techniques September 26 - 28, 2016 Valencia, Spain

Caroline Magnani Spagnol has completed her degree in Biochemistry Pharmacy. She has done her Master’s in Pharmaceutical Sciences and currently pursuing her PhD from São Paulo State University, Brazil. She has published more than 8 papers in reputed journals with 485 reads.

Introduction: The caffeic acid (CA) is a phenolic compound with powerful antioxidant activity. The emulsions are widely used by the consumer; however, preparations developed in the form of dry film are presented as a technological alternative. Aim: The aim of this work was to develop and validate a HPLC method for determination of CA in cosmetic formulations. Methods: HPLC analysis was performed on a Waters™ HPLC with UV-Vis detector, water column RP18 (XDB, 4.6 x 250 mm, 5 μm) ; water: ethanol 60:40 (v/v); pH 2.5 adjusted with acetic acid as mobile phase and flow rate of 0.7 mL min-1 at 325 nm. Results: The method was linear over the concentration range of 10-60 μg/mL (r2=0.9999) with limits of detection and quantification of 1.44 and 4.38 μg/mL, respectively. In the specificity, the peaks obtained with the mobile phase and placebo solution showed no interference in the analysis. Method specificity was also checked by comparing the chromatograms obtained from CA solution in forced degradation procedure and it showed that degradation products did not affect the CA peak. The method was robust, since small changes in the method did not cause significant variations in results. The retention time of CA was 5.9 min. Conclusion: The results indicated that the HPLC method presented linearity, selectivity, accuracy, precision, robustness, adequate detection and quantification limits; with the advantage of having a shorter time compared to existing methods and does not use buffer in the mobile phase. Excellent conditions were chosen in order to obtain a simple and fast HPLC method which can be easily applied in routine analysis of CA in cosmetic formulations.

Barbora Smidova has completed her Master’s degree at Charles University in Prague, Faculty of Pharmacy in 2013. Nowadays, she is in the third year of her PhD study at the same University, Department of Analytical Chemistry. She works at Research and Breeding Institute of Pomology Holovousy, Department of Genebanks as a Junior Researcher. She acquired experiences during two months internship in New Zealand (Massey University) and four months in Portugal (University of Porto). She is author of 1 and a co-author of 5 research papers.

Principal importance of highbush blueberries is mainly in high biological value of fruits. Anthocyanins are the most important pigments of blueberries. Significant property of anthocyanins is their antioxidant activity, which plays important role in prevention of many diseases. A new high-performance liquid chromatography method using alternative pentafluorophenyl fused-core stationary phase has been developed and used for rapid separation of 22 highbush blueberry anthocyanins. High efficiency separation of anthocyanins was achieved on the fused-core column Kinetex PFP, 150 x 4.6 mm (particle size 2.6 µm) protected by precolumn 5 x 4.6 mm. Linear gradient elution with a mobile phase of water solution of 2% formic acid and acetonitrile at a flow rate of 1.0 ml/min was used. The column operated at 50°C and detection wavelength was set at 520 nm. Blueberries were homogenized and extracted with pure methanol, acidified by formic acid using ultrasound water bath for 20 min and immediately filtrated (PTFE, 0.45 μm). 5 µL of sample extract was directly injected into the HPLC system. The developed method has shown efficient separation of 22 anthocyanins in total run time of 21 min. The potential of pentafluorophenyl phase was demonstrated for a wide range of anthocyanins varying in glycosylation and acylation patterns found in highbush blueberries. Described method was applied to 22 highbush blueberry cultivars. Fluorinated stationary phase showed an alternative and complementary separation approach providing unique aromatic and polar selectivity in comparison with common C-18 reversed phases

Kucerova K has completed her Master’s degree from Charles University in Prague at Faculty of Pharmacy in Hradec Kralove. Now, she studies Post-graduate Doctoral Course in Bioanalytical Chemistry at the same faculty. She is interested in liquid chromatography with UV detection and optimization of sample pretreatment.

Ultra-high performance liquid chromatography (UHPLC) presents relatively new technique providing exceptional separation efficiency. Connection of UHPLC with the core-shell particles as a stationary phase is very advantageus. The porous surface of core shell particles allows faster mass transfer and reduce the swirl effect as well as the back pressure of column, UHPLC enables fast and senzitive analyses. The new separation method was developed on KinetexTM C18 column (50 × 2.1 mm) with core-shell particle size of 1.7 µm. The mobile phase was phosphate buffer (25 mM, pH 7.6) and acetonitrile in the ratio 74: 26 (v/v) with total time of analysis 2 minutes and internal calibration. Full validation was performed. The new method was used to monitor the stability of the active substance – omeprazole (proton pump inhibitor) in suspensions and will serve for monitoring of omeprazole stability in individually prepared oral suspensions for pediatric, elderly as well as critically ill patients having problems to wallow solid dosage form.

Maria Vilma obtained her Bachelor and Master of Science degrees in Chemistry from the University of the Philippines, the only state university in the Philippines. She is currently a PhD student at the University of South Australia, Australia. Her research project is on the development of an accurate measurement for petroleum hydrocarbons in soil for risk assessment. She has accumulated many years of experience in R&D, QC, QA, Clinical and manufacturing environments. She is very familiar with laboratory and manufacturing documentation and process systems, having worked within various highly regulated environments that are NATA, TGA or FDA accredited.

Environmental contamination by petroleum hydrocarbons has become a global problem. Due to the complex nature of petroleum components, assessment of the impacted environments has always been based on a risk-based approach that quantifies the total petroleum hydrocarbons (TPHs), instead of measuring the individual fractions. To enhance the TPH analysis, this study examined more feasible fractionation methods for TPHs in contaminated soil using solid phase extraction (SPE) technique followed by analysis utilizing gas chromatography-mass selective detector (GC-MSD) and gas chromatography-flame ionization detector (GC-FID) systems. Present investigation showed an improvement in the separation and quantitation of a total of 31 individual aliphatic components ranging from C10 to C40 and 16 USEPA priority polycyclic aromatic hydrocarbons (PAHs) combined from three different types of soils. The tested adsorbents were silica, florisil and silica/propyl/cyano in commercially available SPE cartridges and traditionally laboratory prepared columns. The silica was found to be the most efficient adsorbent. Parameters that influence the extraction efficiency such as elution solvent, elution volume, breakthrough volume and loading capacity were determined. The accuracy of the aliphatic components ranged from 90.0% to 118.8% with %RSD of 1.4–11.0 with the spiked levels of 1.25, 10.0, 25.0 and 35.0 mg/kg while that of the aromatic components were 61.0–99.0% (%RSD 5.1–9.6) at spiked levels of 1.0, 5.0, 7.0 and 10.0 mg/kg in soil samples. Parameters such as linearity, detection limit and precision were validated. Analysis of the data showed that the present fractionation approach allows much improved

Nehal Fayek Farid has completed her PhD. She is an Assistant Professor of Analytical Chemistry at Faculty of Pharmacy, Beni Suef University. She has published several papers in different chromatographic and spectroscopic methods of analysis and she is a Potential Reviewer in many international journals.

A sensitive, accurate and selective high performance thin layer chromatography HPTLC method was developed and validated for the simultaneous determination of paracetamol (PAR), its toxic impurity 4-aminophenol (4-AP), pseudoephedrine HCl (PSH) and loratidine (LOR). The proposed chromatographic method has been developed using HPTLC aluminum plates precoated with silica gel 60 F254 using acetone: hexane: ammonia (4:5:0.1, by volume) as a developing system followed by densitometric measurement at 254 nm for PAR, 4-AP and LOR, while PSH was scanned at 208 nm. System suitability testing parameters were calculated to ascertain the quality performance of the developed chromatographic method. The method was validated with respect to USP guidelines regarding accuracy, precision and specificity. The method was successfully applied for the determination of paracetamol, pseudoephedrine HCl and loratidine in ATSHI® tablets. The 3 drugs were also determined in plasma by applying the proposed method in the ranges of 0.5-6 µg/band, 1.6-12 µg/band and 0.4-2 µg/band for paracetamol, pseudoephedrine HCl and loratidine, respectively. The results obtained by the proposed method were compared with those obtained by a reported HPLC method; there was no significance difference between both methods regarding accuracy and precision.

Esen Tasgin completed her PhD in 2004 from Ataturk University. She continues to work as an Associate Professor at Ataturk University in Erzurum in Eastern of Turkey. She has published many papers in reputed journals.

It is known that metal oxide nanoparticles have protective effect against ultraviolet photons. Also, they have antioxidant and anti-bacterial effects. In this study, green synthesis of zinc oxide nanoparticles was done with a simple method using peroxidase enzyme and partially purified from fig leaves. The effects of reaction conditions such as optimum pH, temperature and time period were determined. The results showed that ZnO nanoparticles were synthesized in the high yield. The morphological characterization of ZnO nanoparticles were investigated using UV-VIS spectroscopy, scanning electron microscope (SEM) and X-Ray diffraction. Also, antioxidant and antiradicalic activities of ZnO NPs were evaluated. ZnO nanoparticles of antioxidant and radical scavenging activities Fe3+-Fe2+ reduction activity with ferric cyanate reduction method, cupric ions reduction activity with cupric method, Fe3+ reducing capabilities according to the FRAP method, ferrous ions (Fe2+) chelating activity, superoxide anion radical (O2•-) removal activity and 2,2'-Azino-bis(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS•+) radical scavenging activity were determined. BHA and a-tocopherol were used as standard antioxidants in this study. It was determined that ZnO NPs had effective radical reducing activity; and, ZnO NPs were very effective in their radical removal activity and it was also determined to have higher activity than the standard. It was thought that the potential use of ZnO nanoparticles in biomedical and cancer applications is gaining interest in the scientific and medical communities.

Jasmina Agbaba is Full Professor at the Chair of Chemical Technology and Environmental Protection, University of Novi Sad Faculty of Sciences. He received PhD in Chemistry in 2005; MSc in Chemistry in 2000 and BSc in Chemistry Education in 1997 from University of Novi Sad Faculty of Sciences. His research interests include: Water analysis and drinking water treatment, and environmental protection and risk assessment. He has expertise in gas chromatography analysis of environmental samples for wide range of organic pollutants. He has experience of working in laboratory and pilot scale investigations, in particular, relating to applying various drinking water treatment processes. He is Head of the Chair of Chemical Technology and Environmental Protection.

This paper investigates the sorption behavior of As(III) and As(V) on granular activated carbon, quartz sand and zeolite impregnated with Fe–Mn binary oxide (GAC-FeMn, S-FeMn and Z-FeMn). The sorbents was prepared relatively simply by simultaneous oxidation and coprecipitation method. Brunauer-Emmett-Teller (BET) analysis showed that the surface areas of the GAC-FeMn, S-FeMn and Z-FeMn were 996 m2/g, 0.430 m2/g and 55.2 m2/g, respectively. Kinetic experiments (conventional batch technique) were performed with 10 mg of sorbent and 200 µg/l As(III) or As(V) solution at pH 7.0±0.2. In the sorption isotherm study, the adsorbent doses were varied from 0.5-25 g/L, with the same initial As(III) and As(V) concentrations. Pseudo-first order, pseudo-second order, Elowich and intraparticle diffusion models were employed to fit the kinetic data, in order to elucidate the sorption mechanism and potential rate controlling steps such as mass transport and diffusion control processes. The data from the adsorption kinetics best fit with the pseudo-second order model for both As(III) and As(V), suggesting chemical adsorption on the surface of the GAC-FeMn, S-FeMn and Z-FeMn. Intraparticle diffusion model data showed that diffusion was not the only rate-limiting step in the adsorption process. Langmuir and Freundlich models were employed to fit the equilibrium adsorption data, with the Freundlich model giving a better representation, possibly due to irreversible adsorption and the heterogeneous nature of the adsorbents. KF values, rough indicators of sorption capacity, were in the following order: GAC-FeMn>Z-FeMn>S-FeMn for both As(III) and As(V).

Javorska L has completed her Master's degree in 2013 from the Faculty of Pharmacy, Charles University in Prague. Since 2013, she is a PhD student at the Faculty of Pharmacy, Charles University in Prague. She is interested in LC chromatography with UV, FD, MS detection and sample preparation techniques. She has published 1 paper in reputed journal.

Chronic wound is the skin defect persisting longer than 6 weeks or is frequent reoccurrence defect. These wounds remain in a chronic inflammatory state failing a normal healing process patterns. The incidence of the non-healing wounds impaired quality of life for the affected patients and leads to the time-consuming and high cost treatment. The amino acid arginine plays important role in wound healing as the precursor of nitric oxide (NO), proline and polyamines affect all phases of the wound healing process. Monitoring of arginine metabolism directly in the chronic wound could be another indicator of the chronic wound healing process and significantly improve the therapy. Our HPLC method with fluorescence detection enable determination of arginine, ornithine and citrulline in a fluid obtained from chronic wounds. Separation of amino acids was performed using C18 monolithic HPLC column. Sodium acetate buffer (solution A) and mixture of ACN and MeOH (solution B) were used as the mobile phase in gradient elution mode. Total time of analysis was 14 min including the column-wash step. The method was validated by testing its linearity, precision, accuracy, recovery, robustness and detection limit/quantitation limit values. This method will be used for clinical research of the chronic wound healing process.

Nada Sayed Abdelwahab has completed her PhD. She is an Associate Professor of Analytical Chemistry at Faculty of Pharmacy Beni Suef University. She has published more than 40 papers in different chromatographic and spectroscopic methods of analysis. She also attended different international conferences and is a Potential Reviewer in many international journals.

An isocratic RP-HPLC-DAD method has been developed and optimized for the first time by the aid of statistical approaches for simultaneous determination of acemetacin (ACM) and its official impurities (A and B), 4- chlorobenzoic acid (IMP-A) and indometacin (IMP-B). In this study, two level full factorial design was used to optimize the used mobile phase where three chromatographic variables were studied, % acetonitrile (ACN), % H3PO4 acid and mobile phase flow rate (FR). The selected responses were the analysis time (t) and the chromatographic resolution (Rs) among the most adjacent peaks (peaks IMP-B and ACM). The impacts of % acetonitrile and mobile phase flow rate individually were significant on analysis time (P=0.0277 and 0.0424, respectively). Also %acetonitrile had a meaningful effect on the chromatographic resolution (P=0.0085). Finally the chromatographic separation has been performed on Zorbax® Eclipse C18 column using acetonitrile: Water (containing 0.05% H3PO4) [55:45, v/v], FR=1.5 mL/min as an optimized mobile phase using full factorial experimental design with UV detection at 230nm. IMP-A appeared at 3.29 minute, IMP-B at 9.07 minute and ACM at 10 minutes. The method fulfilled USP validation standards concerning linearity, accuracy and precision. In addition, system suitability parameters have been calculated and the results were within the acceptance criteria. The commercially available ACM tablets were analyzed, good %recovery and %RSD values were resulted. Also, statistical comparison of the developed method with the reported one showed no significant difference within probability of 95%.

Haochun Tang received the BS degree in Mechanical Engineering from Chun Yuan Christian University, Taoyuan, Taiwan, in 2011. He received the MS degree in Innovative and Engineered Materials from Tokyo Institute of Technology, Yokohama, Japan, in 2015, and is currently working towards the PhD degree in Materials Science and Engineering at Tokyo Institute of Technology. His research interests include the effects of supercritical carbon dioxide in electrodeposition of metallic materials.

Gold materials are often used in the electronic industry due to their high chemical stability, corrosion resistance, electrical conductivity and density. Electrodeposition (ECD) has been wildely employed in preparation of Au materials for micro-electrical-mechanical system (MEMS) devices, i.e. capacitive accelerometer. However, mechanical strength of Au materials is relatively low when compared with other matallic materials, which is often a concern in practical applications in MEMS. In previous studies, grain refinement effect was observed in nickel films prepared by ECD with the electrolyte containing supercritical carbon dioxide (scCO2), which resulted a significant enhancement in the mechanical properties according to Hall-Petch relation. In this work, the ECD with scCO2 (ECD-scCO2) was applied in fabrication of Au materials, and the micro-mechanical properties were evaluated. Two kinds Au films with 50 m thickness were first prepared by the ECD with sulfite-based Au electrolyte: One is conventional ECD (ECD-CONV) without employing the scCO2; the other is ECD-scCO2. Micro-pillars were fabricated from the Au films by focus ion beam (FIB) milling, where the pillar size was fixed at 15 m  15 m  30 m (aspect ratio is 2). Micro-compression tests were carried out using a testing machnine specially designed in our group. For the ECD-scCO2, a compressive strength of ~800 Mpa was obtained, which is far larger than the ECD-CONV pillar (500 MPa). The results indicated that employing scCO2 in the Au ECD process is effective in enhancing the mechanical properties of the Au materials.

Jeon Hoon Kim has completed his PhD in KAIST, Korea in 1999 and Post-doctoral studies from Department of Chemical Engineering from Waterloo University, Canada in 2000. He is Head of Greenhouse Gas Separation and Recovery Group in KRICT, Korea. He has published more than 90 papers in reputed journals and has been serving as Executive Director in The Membrane Society of Korea.

In petrochemical process, catalytic cracking of naphtha (NCC) process requires extremely high energy consumption for separation of ethylene from ethane or propylene from propane mixtures by low-temperature distillation. Membrane-based gas separation enables these separation processes to be low-energy consuming and environment friendly, if high olefin selective membrane materials. Facilitated transport membranes (FTM) have been known to show very high olefin selectivity over paraffin. This study is aimed to develop the membrane materials and show their separation properties for propylene and propane. We prepared FTM module using PVP/AgBF4/TCNQ composite membrane on top of hollow fiber membrane. Pure gases and mixed gas permeation test were performed in various operational conditions. We developed simulation program predicting the membrane separation properties under operation conditions. Separation properties of FTM module for propylene and propane were obtained from the simulation program based on the pure gas permeation data. The FTM showed high propylene/propane selectivity and propylene permeabilities. It is predicted that one-stage or two-stage membrane process provides over 99.5% of propylene at permeate side at high propylene recovery from a binary gas mixture of 95 vol% C3H6/5 vol% C3H8 supplied as a feed gas. The results showed FT membranes could be effectively used in C3 separation process instead of typical NCC (Naphtha Cracking Center) C3 splitter.