Search results for: planar chromatography

Authors: Sumonthip Kongtun Janphuk

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Ten cereal grains that usually used as ingredients in healthy products were studied for phytosteryl glucoside contents. β-sitosteryl glucoside in 10 cereal grains, including Phasecolus vulgaris L. (kidney bean), Sorghum bicolor (sorghum), Moringa oleifera Lam. (drumstick), Nelumbo nucifera (lotus), Vigna radiate L. (mung bean), Coix lacrymajobi (job’tears), Oryza sativa. (red rice), Glycine max L. Merrill. (soybean),Cucurbita maschata Decne (pumpkin) and Helianthas annuus (sunflower seeds), were analyzed using Thin-layer chromatography (TLC) and High-Performance liquid chromatography (HPLC). All grains were extracted with methanol before analysis. Red bean showed the maximum phytosteryl glucoside content of 0.42% w/w. The content of others were as follows: pumpkin seed 0.173%, mung bean 0.099 %, soybean 0.07%, dried moringa seed 0.067%, lotus seed 0.044%, sorghum 0.032%, sunflower seed 0.016%, Job's tears 0.012%, and brown rice 0.006%.

Keywords: cereal grains, phytosterol, β-sitosteryl glucoside, food analysis.

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Authors: Nabil Jallouli, Luisa M. Pastrana-Martínez, Ana R. Ribeiro, Nuno F. F. Moreira, Joaquim L. Faria, Olfa Hentati, Adrián M. T. Silva, Mohamed Ksibi

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Degradation and mineralization of ibuprofen (IBU) were investigated using Ultraviolet (UV) Light Emitting Diodes (LEDs) in TiO2 photocatalysis. Samples of ultrapure water (UP) and a secondary treated effluent of a municipal wastewater treatment plant (WWTP), both spiked with IBU, as well as a highly concentrated IBU (230 mgL-1) pharmaceutical industry wastewater (PIWW), were tested in the TiO2/UV-LED system. Three operating parameters, namely, pH, catalyst load and number of LEDs were optimized. The process efficiency was evaluated in terms of IBU removal using high performance liquid chromatography (HPLC) and ultra-high performance liquid chromatography coupled to tandem mass spectrometry (UHPLC-MS/MS). Additionally, the mineralization was investigated by determining the dissolved organic carbon (DOC) content. The chemical structures of transformation products were proposed based on the data obtained using liquid chromatography with a high resolution mass spectrometer ion trap/time-of-flight (LC-MS-IT-TOF). A possible pathway of IBU degradation was accordingly proposed. Bioassays were performed using the marine bacterium Vibrio fischeri to evaluate the potential acute toxicity of original and treated wastewaters. TiO2 heterogeneous photocatalysis was efficient to remove IBU from UP and from PIWW, and less efficient in treating the wastewater from the municipal WWTP. The acute toxicity decreased by ca. 40% after treatment, regardless of the studied matrix.

Keywords: acute toxicity, Ibuprofen, UV-LEDs, wastewaters

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Authors: Emmanuel O Ajani, Sabiu S, Mariam Zakari, Fisayo A Bamisaye

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Hydrocotyl bonariensis is a plant which anticataractogenic potentials have been reported. In the present study an attempt was made to evaluate the in vitro antioxidant activity of the fractionates of the leaves extract and also characterize some of its chemical constituents. DPPH, H₂O₂, OH and NO free radical scavenging, metal chelating and reducing power activity was used to evaluate the antioxidant activity of the crude extract fractionates. Fresh leaves of Hydrocotyl bonariensis leaves were extracted in 70% methanol. The extract was partitioned with different solvent system of increasing polarity (n-hexane, chloroform, ethyl acetate methanol and water). Compounds were isolated from the aqueous practitionate using accelerated gradient chromatography, vacuum liquid chromatography, preparative TLC and conventional column chromatography. The presence of the chemical groups was established with HPLC and Fourier Transform Infra Red. The structures of isolated compounds were elucidated by spectroscopic study and chemical shifts. Data from the study indicates that all the fractionates contain compounds with free radical scavenging activity. This activity was more pronounced in the aqueous fractionate (DPPH IC₅₀, 0025 ± 0.011 mg/ml, metal chelating capacity 27.5%, OH- scavenging IC₅₀, 0.846 ± 0.037 mg/ml, H₂O₂ scavenging IC₅₀ 0.521 ± 0.015 mg/ml, reducing power IC₅₀ 0.248 ± 0.025 mg/ml and NO scavenging IC₅₀ 0.537 ± 0.038 mg/ml). Two compounds were isolated and when compared with data from the literature; the structures were suggestive of polyphenolic flavonoid, quercetin and 3-O-β-D-glucopyranosyl-sitosterol. The result indicates that H. bonariensis leaves contain bioactive compounds with antioxidant activity.

Keywords: antioxidant, cataract, free radical, flavonoids, hydrocotyl bonariensis

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Authors: Abubakar Sani

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The leaves extracts of Cassia sieberiana D.C. were screened for cytotoxicity using Brine Shrimp Test (BST) and antimicrobial bioassay against Staphylococcus aureus, Salmonella typhi and Escherichia coli using crude ethanol extract, Chloroform soluble fraction, aqueous soluble fraction, ethyl acetate soluble fraction, methanol soluble fraction and n-hexane soluble fraction. The Ethyl acetate fraction obtained proved to be most active in inducing complete lethality at minimum doses in BST and also active on Salmonella typhi. The Bioactivity result was used to guide the column chromatography which led to the isolation of pure compound CSB-8 which was found active in the BST with LC₅₀ value of 34(722-182)µg/ml and showed remarkable activity on Salmonella typhi (zone of inhibition 25mm) at 10,000µg/ml. The ¹H-NMR, ¹³C NMR, FTIR and GC-MS spectra of compound suggested the proposed structure to be 2-pentadecanone.

Keywords: brine shrimp, Cassia sieberiana D. C, Column chromatography, antimicrobial bioassay

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Authors: Anil P. Dewani, Alok S. Tripathi, Anil V. Chandewar

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Present manuscript reports the development and validation of a quantitative high performance liquid chromatography method for the pharmacokinetic evaluation of Glimepiride (GLM) and Ilaprazole (ILA) in rat plasma. The plasma samples were involved with Solid phase extraction process (SPE). The analytes were resolved on a Phenomenex C18 column (4.6 mm× 250 mm; 5 µm particle size) using a isocratic elution mode comprising methanol:water (80:20 % v/v) with pH of water modified to 3 using Formic acid, the total run time was 10 min at 225 nm as common wavelength, the flow rate throughout was 1ml/min. The method was validated over the concentration range from 10 to 600 ng/mL for GLM and ILA, in rat plasma. Metformin (MET) was used as Internal Standard. Validation data demonstrated the method to be selective, sensitive, accurate and precise. The limit of detection was 1.54 and 4.08 and limit of quantification was 5.15 and 13.62 for GLM and ILA respectively, the method demonstrated excellent linearity with correlation coefficients (r2) 0.999. The intra and inter-day precision (RSD%) values were < 2.0% for both ILA and GLM. The method was successfully applied in pharmacokinetic studies followed by oral administration in rats.

Keywords: pharmacokinetics, glimepiride, ilaprazole, HPLC, SPE

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Authors: Yuta Tachibana, Ayuko Itsuki

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The three strains of bacteria (Lysinibacillus xylanilyticus, Bacillus kochii, and Enterococcus sp.) were isolated from the fermented Indigo (Polygonum tinctorium) dyeing solution using the dilution plate method and some fermentation conditions were determined. High-Performance Liquid Chromatography (HPLC) was used to determine the indigo concentration. When the isolated bacteria were cultured in the indigo liquid culture containing various sugars, starch, and ethanol, the indigo culture solutions containing galactose, mannose, ribose, and ethanol were remarkably decreased. Comparison of decreasing indigo between three strains showed that Enterococcus sp. had the fastest growth and decrease of indigo. However, decreasing indigo per unit micro biomass did not correspond to the results of decreasing indigo―Bacillus kochii had higher indigo-reducing activity than Enterococcus sp. and Lysinibacillus xylanilyticus.

Keywords: fermentation condition, high-performance liquid chromatography (HPLC), indigo dyeing solution, indigo-reducing activity

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Authors: Ghasem Khodahami, Vahid Rowshan, Mojtaba Pakparvar

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Stachys forms one of the largest genera in the flowering plant family Lamiaceae. The number of species in the genus is estimated from about 300 to about 450 and comprises some 34 species in Iran. This genus is one of the richest sources of diterpenes which are particularly interesting because of their ecological role as antifeedants against different species of insects and for their role as the medicinal properties of the plants. The ecological distribution of Stachys inflata was studied and the resulted eco-types were sampled from four regions ranging 230-340 mm of rainfall and 1690-2125 m a.s.l of height In Fars Province Southern Iran. The essential oils of air-dried samples were obtained by hydrodistillation and analyzed by gas chromatography and gas chromatography/mass spectrometry. The number of secondary metabolites varied from 25 to 50 depending to ecological conditions. The main compounds in these areas were: Germacrene D, Bicyclogermacrene, spathulenol, δ-cadinene. Statistical analysis of photochemical resulted in recognizing 3 distinct groups that show internal variety in these herbs.

Keywords: eco-type, phytochemistry, secondary metabolites, Stachys inflata

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Authors: Bong Keun Kang, Sung Suk Oh, Jeong-Woo Sohn, Jong-Ryul Choi, Young Ho Kim

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In this paper, we describe two-step micro-pattering by using laser cutting and wax printing. Wax printing is performed only on the bridges for hydrophobic barriers. We prepared 405nm blue-violet laser module and wax pencil module. And, this two modules combine x-y plot. The hollow microstructure formed by laser patterning define the hydrophilic flowing paths. However, bridges are essential to avoid the cutting area being the island. Through the support bridges, microfluidic solution spread out to the unnecessary areas. Chromatography blotting paper was purchased from Whatman. We used 20x20 cm and 46x57 cm of chromatography blotting paper. Axis moving speed of x-y plot was the main parameter of optimization. For aligning between the two patterning, the paper sheet was taped at the bottom. After the two-step patterning, temperature curing step was done at 110-130 °C. The resolution of the fabrication and the potential of the multiplex detection were investigated.

Keywords: µPADs, microfluidic, biosensor, mass-fabrication

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Authors: Jyh Sheen, Yang-Hung Cheng

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This paper presents a design of a microstrip bandpass filter with a compact size and wide stopband by using 0.15-μm GaAs pHEMT process. The wide stop band is achieved by suppressing the first and second harmonic resonance frequencies. The slow-wave coupling stepped impedance resonator with cross coupled structure is adopted to design the bandpass filter. A two-resonator filter was fabricated with 13.5GHz center frequency and 11% bandwidth was achieved. The devices are simulated using the ADS design software. This device has shown a compact size and very low insertion loss of 2.6 dB. Microstrip planar bandpass filters have been widely adopted in various communication applications due to the attractive features of compact size and ease of fabricating. Various planar resonator structures have been suggested. In order to reach a wide stopband to reduce the interference outside the passing band, various designs of planar resonators have also been submitted to suppress the higher order harmonic frequencies of the designed center frequency. Various modifications to the traditional hairpin structure have been introduced to reduce large design area of hairpin designs. The stepped-impedance, slow-wave open-loop, and cross-coupled resonator structures have been studied to miniaturize the hairpin resonators. In this study, to suppress the spurious harmonic bands and further reduce the filter size, a modified hairpin-line bandpass filter with cross coupled structure is suggested by introducing the stepped impedance resonator design as well as the slow-wave open-loop resonator structure. In this way, very compact circuit size as well as very wide upper stopband can be achieved and realized in a Roger 4003C substrate. On the other hand, filters constructed with integrated circuit technology become more attractive for enabling the integration of the microwave system on a single chip (SOC). To examine the performance of this design structure at the integrated circuit, the filter is fabricated by the 0.15 μm pHEMT GaAs integrated circuit process. This pHEMT process can also provide a much better circuit performance for high frequency designs than those made on a PCB board. The design example was implemented in GaAs with center frequency at 13.5 GHz to examine the performance in higher frequency in detail. The occupied area is only about 1.09×0.97 mm2. The ADS software is used to design those modified filters to suppress the first and second harmonics.

Keywords: microstrip resonator, bandpass filter, harmonic suppression, GaAs

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Authors: Rajesh S. Mony, Vaidyaratnam Oushadhasala

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An attempt is made in this study to evolve a drug development modality based on classical Ayurvedic knowledge base as well as on modern scientific methodology. The present study involves (a) identification of a specific ailment condition, (b) the selection of a polyherbal formulation, (c) deciding suitable extraction procedure, (d) confirming the efficacy of the combination by in-vitro trials and (e) fixing up the recommended dose. The ailment segment selected is arthritic condition. The selected herbal combination is Kunturushka, Vibhitaki, Guggulu, Haridra, Maricha and Nirgundi. They were selected as per Classical Ayurvedic references, Authentified as per API (Ayurvedic Pharmacopeia of India), Extraction of each drug was done by different ratios of Hydroalcoholic menstrums, Invitro assessment of each extract after removing residual solvent for anti-Inflammatory, anti-arthritic activities (by UV-Vis. Spectrophotometer with positive control), Invitro assessment of each extract for COX enzyme inhibition (by UV-Vis. Spectrophotometer with positive control), Selection of the extracts was made having good in-vitro activity, Performed the QC testing of each selected extract including HPTLC, that is the in process QC specifications, h. Decision of the single dose with mixtures of selected extracts was made as per the level of in-vitro activity and available toxicology data, Quantification of major groups like Phenolics, Flavonoids, Alkaloids and Bitters was done with both standard Spectrophotometric and Gravimetric methods, Method for Marker assay was developed and validated by HPTLC and a good resolved HPTLC finger print was developed for the single dosage API (Active Pharmaceutical Ingredient mixture of extracts), Three batches was prepared to fix the in process and API (Active Pharmaceutical Ingredient) QC specifications.

Keywords: drug development, antiinflammatory, quality stardardisation, planar chromatography

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Authors: Abid Fida Masih

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Forced degradation study of Rifaximin was conducted to determine the stability indicating potential of HPLC testing method for detection of Rifaximin in formulated tablets to be employed for quality control and stability testing. The questioned method applied with mobile phase methanol: water (70:30), 5µm, 250 x 4.6mm, C18 column, wavelength 293nm and flow rate of 1.0 ml/min. Forced degradation study was performed under oxidative, acidic, basic, thermal and photolytic conditions. The applied method successfully determined the degradation products after acidic and basic degradation without interfering with Rifaximin detection. Therefore, the method was said to be stability indicating and can be applied for quality control and stability testing of Rifaxmin tablets during its shelf life.

Keywords: forced degradation, high-performance liquid chromatography, method validation, rifaximin, stability indicating method

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Authors: Ferhat Mohamed, Boukhatem Mohamed Nadjib, Chemat Farid

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Simultaneous distillation–extraction (SDE) is routinely used by analysts for sample preparation prior to gas chromatography analysis. In this work, a new process design and operation for microwave assisted simultaneous distillation – solvent extraction (MW-SDE) of volatile compounds was developed. Using the proposed method, isolation, extraction and concentration of volatile compounds can be carried out in a single step. To demonstrate its feasibility, MW-SDE was compared with the conventional technique, Simultaneous distillation–extraction (SDE), for gas chromatography-mass spectrometry (GC-MS) analysis of volatile compounds in a fresh orange juice and a dry spice “carvi seeds”. SDE method required long time (3 h) to isolate the volatile compounds, and large amount of organic solvent (200 mL of hexane) for further extraction, while MW-SDE needed little time (only 30 min) to prepare sample, and less amount of organic solvent (10 mL of hexane). These results show that MW-SDE–GC-MS is a simple, rapid and solvent-less method for determination of volatile compounds from aromatic plants.

Keywords: essential oil, extraction, distillation, carvi seeds

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Authors: Asmat Nawaz, Ceylan Zafer, Ali K. Erdinc, Kaiying Wang, M. Nadeem Akram

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Hybrid halide Perovskites with the general formula ABX₃, where X = Cl, Br or I, are considered as an ideal candidates for the preparation of photovoltaic devices. The most commonly and successfully used hybrid halide perovskite for photovoltaic applications is CH₃NH₃PbI₃ and its analogue prepared from lead chloride, commonly symbolized as CH₃NH₃PbI₃_ₓClₓ. Some researcher groups are using lead free (Sn replaces Pb) and mixed halide perovskites for the fabrication of the devices. Both mesoporous and planar structures have been developed. By Comparing mesoporous structure in which the perovskite materials infiltrate into mesoporous metal oxide scaffold, the planar architecture is much simpler and easy for device fabrication. In a typical perovskite solar cell, a perovskite absorber layer is sandwiched between the hole and electron transport. Upon the irradiation, carriers are created in the absorber layer that can travel through hole and electron transport layers and the interface in between. We fabricated inverted planar heterojunction structure ITO/PEDOT/ Perovskite/PCBM/Al, based solar cell via two-step spin coating method. This is also called Sequential deposition method. A small amount of cheap additive H₂O was added into PbI₂/DMF to make a homogeneous solution. We prepared four different solution such as (W/O H₂O, 1% H₂O, 2% H₂O, 3% H₂O). After preparing, the whole night stirring at 60℃ is essential for the homogenous precursor solutions. We observed that the solution with 1% H₂O was much more homogenous at room temperature as compared to others. The solution with 3% H₂O was precipitated at once at room temperature. The four different films of PbI₂ were formed on PEDOT substrates by spin coating and after that immediately (before drying the PbI₂) the substrates were immersed in the methyl ammonium iodide solution (prepared in isopropanol) for the completion of the desired perovskite film. After getting desired films, rinse the substrates with isopropanol to remove the excess amount of methyl ammonium iodide and finally dried it on hot plate only for 1-2 minutes. In this study, we added H₂O in the PbI₂/DMF precursor solution. The concept of additive is widely used in the bulk- heterojunction solar cells to manipulate the surface morphology, leading to the enhancement of the photovoltaic performance. There are two most important parameters for the selection of additives. (a) Higher boiling point w.r.t host material (b) good interaction with the precursor materials. We observed that the morphology of the films was improved and we achieved a denser, uniform with less cavities and almost full surface coverage films but only using precursor solution having 1% H₂O. Therefore, we fabricated the complete perovskite solar cell by sequential deposition technique with precursor solution having 1% H₂O. We concluded that with the addition of additives in the precursor solutions one can easily be manipulate the morphology of the perovskite film. In the sequential deposition method, thickness of perovskite film is in µm and the charge diffusion length of PbI₂ is in nm. Therefore, by controlling the thickness using other deposition methods for the fabrication of solar cells, we can achieve the better efficiency.

Keywords: methylammonium lead iodide, perovskite solar cell, precursor composition, sequential deposition

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Authors: Furqan M. Kadhum, Asmaa A. Hussein, Maysaa Ch. Hatem

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Hyaluronidase enzyme was purified from the clinical isolate Staphyloccus aureus in three purification steps, first by precipitation with 90% saturated ammonium sulfate, ion exchange chromatography on DEAE-Cellulose, and gel filtration chromatography throughout Sephacryl S-300. Specific activity of the purified enzyme was reached 930 U/mg protein with 7.4 folds of purification and 46.5% recovery. The enzyme has an average molecular weight of about 69 kDa, with an optimum pH of enzyme activity and stability at pH 7, also the optimum temperature for activity was 37oC. The enzyme was stable with full activity at a temperature ranged between 30-40 oC. Metal ions showed variable inhibitory degree with the strongest effect for Fe+3, however, the chelating and reducing agents had no or little effects. Cytotoxic studies for purified and crude hyaluronidase against cancer cell Hep G2 type at different enzyme concentrations and exposure times showed that the inhibition effect of both crude and purified enzyme increased by increasing the enzyme concentration with no change was observed at 24hr, while at 48 and 72 hrs the same inhibition rate were observed for purified enzyme and differ for the crude filtrate.

Keywords: hyaluronidase, S. aureus, metal ions, cytotoxicity

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Authors: Birute Bugelyte, Ingrida Jurkute, Vida Vickackaite

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The most complicated step of the determination of volatile compounds in complex matrices is the separation of analytes from the matrix. Traditional analyte separation methods (liquid extraction, Soxhlet extraction) require a lot of time and labour; moreover, there is a risk to lose the volatile analytes. In recent years, headspace gas chromatography has been used to determine volatile compounds. To date, traditional extraction solvents have been used in headspace gas chromatography. As a rule, such solvents are rather volatile; therefore, a large amount of solvent vapour enters into the headspace together with the analyte. Because of that, the determination sensitivity of the analyte is reduced, a huge solvent peak in the chromatogram can overlap with the peaks of the analyts. The sensitivity is also limited by the fact that the sample can’t be heated at a higher temperature than the solvent boiling point. In 2018 it was suggested to replace traditional headspace gas chromatographic solvents with non-volatile, eco-friendly, biodegradable, inexpensive, and easy to prepare deep eutectic solvents (DESs). Generally, deep eutectic solvents have low vapour pressure, a relatively wide liquid range, much lower melting point than that of any of their individual components. Those features make DESs very attractive as matrix media for application in headspace gas chromatography. Also, DESs are polar compounds, so they can be applied for microwave assisted extraction. The aim of this work was to investigate the possibility of applying deep eutectic solvents for microwave assisted extraction and headspace gas chromatographic determination of hexanal in fat-rich food. Hexanal is considered one of the most suitable indicators of lipid oxidation degree as it is the main secondary oxidation product of linoleic acid, which is one of the principal fatty acids of many edible oils. Eight hydrophilic and hydrophobic deep eutectic solvents have been synthesized, and the influence of the temperature and microwaves on their headspace gas chromatographic behaviour has been investigated. Using the most suitable DES, microwave assisted extraction conditions and headspace gas chromatographic conditions have been optimized for the determination of hexanal in potato chips. Under optimized conditions, the quality parameters of the prepared technique have been determined. The suggested technique was applied for the determination of hexanal in potato chips and other fat-rich food.

Keywords: deep eutectic solvents, headspace gas chromatography, hexanal, microwave assisted extraction

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Authors: Luke Andrighetto, Paul G. Stevenson, Luke C. Henderson, Jim Pearson, Xavier A. Conlan

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As pseudoephedrine, a common ingredient in cold and flu medications is closely monitored and restricted in Australia, alternative methods of accessing it are of interest. The impurities and by-products of every reaction step of pseudoephedrine/ephedrine and methamphetamine synthesis have been mapped in order to develop a chemical fingerprint based on synthetic route. Likewise, seized methamphetamine contains a combination of different cutting agents and starting materials. Therefore, in-silico optimised two-dimensional HPLC with DryLab® and OpenMS® software has been used to efficiently separate complex seizure samples. An excellent match between simulated and real separations was observed. Targeted separation of model compounds was completed with significantly reduced method development time. This study produced a two-dimensional separation regime that offers unprecedented separation power (separation space) while maintaining a rapid analysis time that is faster than those previously reported for gas chromatography, single dimension high performance liquid chromatography or capillary electrophoresis.

Keywords: chemical fingerprint, ephedrine, methamphetamine, two-dimensional HPLC

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Authors: H. M. El-Rafie, A. H. Abou Zeid, R. S. Mohammed, A. A. Sleem

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Acrocarpus is a genus of flowering plants in the legume family Fabaceae which considered as a large and economically important family. This study aimed to investigate the phytoconstituents of the petroleum ether extract (PEE) of Acrocarpus fraxinofolius bark by Gas chromatography coupled with mass spectrometry (GC/MS) analysis of its fractions (fatty acid and unsaponifiable matter). Concerning this, identification of 52 compounds constituting 97.03 % of the total composition of the unsaponifiable matter fraction. Cycloeucalenol was found to be the major compound representing 32.52% followed by 4a, 14a-dimethyl-A8~24(28)-ergostadien (26.50%) and ß-sitosterol(13.74%), furthermore Gas liquid chromatography (GLC) analysis of the sterol fraction revealed the identification of cholesterol (7.22 %), campesterol (13.30 %), stigmasterol (10.00 %) and β - sitosterol (69.48 %). Meanwhile, the identification of 33 fatty acids representing 90.71% of the total fatty acid constituents. Methyl-9,12-octadecadienoate (40.39%) followed by methyl hexadecanoate (23.64%) were found to be the major compounds. On the other hand, column chromatography and Thin layer chromatography (TLC) fractionation of PEE separate the triterpenoid: 21β-hydroxylup-20(29)-en-3-one and β- amyrin which were structurally identified by spectroscopic analysis (NMR, MS and IR). PEE has been biologically evaluated for 1: management of diabetes in alloxan induced diabetic rats 2: cytotoxic activity against four human tumor cell lines (Cervix carcinoma cell line[HELA], Breast carcinoma cell line [MCF7], Liver carcinoma cell line[HEPG2] and Colon carcinoma cell line[HCT-116] 3: hepatoprotective activity against CCl4-induced hepatotoxicity in rats and the activity was studied by assaying the serum marker enzymes like AST, ALT, and ALP. Concerning this, the anti-diabetic activity exhibited by 100mg of PEE extract was 74.38% relative to metformin (100% potency). It also showed a significant anti-proliferative activity against MCF-7 (IC50= 2.35µg), Hela(IC50=3.85µg) and HEPG-2 (IC50= 9.54µg) compared with Doxorubicin as reference drug. The hepatoprotective activity was evidenced by significant decrease in liver function enzymes, i.e. AST, ALT and ALP by (29.18%, 28.26%, and 34.11%, respectively using silymarin as the reference drug, compared to their concentration levels in an untreated group with liver damage induced by CCl₄. This study was performed for the first time on the bark of this species.

Keywords: Acrocarpus fraxinofolius, antidiabetic, cytotoxic, hepatoprotective

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Authors: Li Feng, Cheng Zhang, Chuanzhou Yuang

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Understanding the macromolecular structure of low-rank coal is very important for its gasification and liquefaction. The pyrolysis is one of the methods of analyzing the macromolecular structure of coal. The gaseous products decomposed directly by the raw lignite at 500 °C and indirectly by tar products from raw lignite pyrolysis at 500 °C were investigated and compared by thermogravimetry, gas chromatography and mass spectrum coupled instrument system (TG/GC/MS) in this paper. The results show that 52 kinds of products were found from the raw lignite and 70 kinds of products from the tar. The pyrolysis products directly from the lignite appear more monocyclic aromatic hydrocarbons and less substituent groups or branch chain, compared with the products from the tar. There is less linear chain and double bonds structure in the tar, which can be speculated that linear chain and double bonds structure took part in the generation of condensed rings and other reactions. There are more kinds of phenol and furan in the tar, which indicate that these products may be generated from the secondary reaction. The formation process of phenol, phenol naphthalene, naphthene and furan are discussed.

Keywords: composition and structure, lignite, pyrolysis of coal, tar, TG/GC/MS

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Authors: Narayana Murthy Akurathi, Vijaya Lakshmi Marella

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The literature is reviewed with regard to online Super critical fluid extraction (SFE) coupled directly with supercritical fluid chromatography (SFC) -mass spectrometry that have typically more sensitive than conventional LC-MS/MS and GC-MS/MS. It is becoming increasingly interesting to use on-line techniques that combine sample preparation, separation and detection in one analytical set up. This provides less human intervention, uses small amount of sample and organic solvent and yields enhanced analyte enrichment in a shorter time. The sample extraction is performed under light shielding and anaerobic conditions, preventing the degradation of thermo labile analytes. It may be able to analyze compounds over a wide polarity range as SFC generally uses carbon dioxide which was collected as a by-product of other chemical reactions or is collected from the atmosphere as it contributes no new chemicals to the environment. The diffusion of solutes in supercritical fluids is about ten times greater than that in liquids and about three times less than in gases which results in a decrease in resistance to mass transfer in the column and allows for fast high resolution separations. The drawback of SFC when using carbon dioxide as mobile phase is that the direct introduction of water samples poses a series of problems, water must therefore be eliminated before it reaches the analytical column. Hundreds of compounds analysed simultaneously by simple enclosing in an extraction vessel. This is mainly applicable for pharmaceutical industry where it can analyse fatty acids and phospholipids that have many analogues as their UV spectrum is very similar, trace additives in polymers, cleaning validation can be conducted by putting swab sample in an extraction vessel, analysing hundreds of pesticides with good resolution.

Keywords: super critical fluid extraction (SFE), super critical fluid chromatography (SFC), LCMS/MS, GCMS/MS

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Authors: Aniqa Jabeen

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The aim of this study was to evaluate the effectiveness of Tc-99m MIBI (Technetium 99-methoxy-iso-butyl-isonitrile) scintigraphy to differentiate malignancies from benign lesions, which were detected on planar bone scans. Materials and Methods: 59 patients with bone lesions were enrolled in the study. The scintigraphic findings were compared with the clinical, radiological and the histological findings. Each patient initially underwent a three-phase bone scan with Tc-99m MDP (Methylene Diphosphonate) and if evidence of lesion found, the patient then underwent a dynamic and static MIBI scintigraphy after three to four days. The MDP and MIBI scans were evaluated visually and quantitatively. For quantitative analysis count ratios of lesions and contralateral normal side (L/C) were taken by region of interests drawn on scans. The Student T test was applied to assess the significant difference between benign and malignant lesions p-value < 0.05 was considered significant. Result: The MDP scans showed the increase tracer uptake, but there was no significant difference between benign and malignant uptake of the radiotracer. However significant difference (p-value 0.015), in uptake was seen in malignant (L/C = 3.51 ± 1.02) and benign lesion (L/C = 2.50±0.42) on MIBI scan. Three of thirty benign lesions did not show significant MIBI uptake. Seven malignant appeared as false negatives. Specificity of the scan was 86.66%, and its Negative Predictive Value (NPV) was 81.25% whereas the sensitivity of scan was 79.31%. In excluding the axial metastasis from the lesions, the sensitivity of MIBI scan increased to 91.66% and the NPV also increased to 92.85%. Conclusion: MIBI scintigraphy provides its usefulness by distinguishing malignant from benign lesions. MIBI also correctly identifies metastatic lesions. The negative predictive value of the scan points towards its ability to accurately diagnose the normal (benign) cases. However, biopsy remains the gold standard and a definitive diagnostic modality in musculoskeletal tumors. MIBI scan provides useful information in preoperative assessment and in distinguishing between malignant and benign lesions.

Keywords: benign, malignancies, MDP bone scan, MIBI scintigraphy

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Authors: Nader Nciri, Suil Song, Namho Kim, Namjun Cho

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Properties and compositions of bitumen and bitumen-derived liquids have significant influences on the selection of recovery, upgrading and refining processes. Optimal process conditions can often be directly related to these properties. The end uses of bitumen and bitumen products are thus related to their compositions. Because it is not possible to conduct a complete analysis of the molecular structure of bitumen, characterization must be made in other terms. The present paper focuses on physico-chemical analysis of two different types of bitumens. These bitumen samples were chosen based on: the original crude oil (sand oil and crude petroleum), and mode of process. The aim of this study is to determine both the manufacturing effect on chemical species and the chemical organization as a function of the type of bitumen sample. In order to obtain information on bitumen chemistry, elemental analysis (C, H, N, S, and O), heavy metal (Ni, V) concentrations, IATROSCAN chromatography (thin layer chromatography-flame ionization detection), FTIR spectroscopy, and 1H NMR spectroscopy have all been used. The characterization includes information about the major compound types (saturates, aromatics, resins and asphaltenes) which can be compared with similar data for other bitumens, more importantly, can be correlated with data from petroleum samples for which refining characteristics are known. Examination of Asphalt Ridge froth bitumen showed that it differed significantly from representative petroleum pitches, principally in their nonhydrocarbon content, heavy metal content and aromatic compounds. When possible, properties and composition were related to recovery and refining processes. This information is important because of the effects that composition has on recovery and processing reactions.

Keywords: froth bitumen, oil sand, asphalt ridge, petroleum pitch, thin layer chromatography-flame ionization detection, infrared spectroscopy, 1H nuclear magnetic resonance spectroscopy

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Authors: F. Mutelet, L. Cesari

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Development of safer and environmentally friendly processes and products is needed to achieve sustainable production and consumption patterns. Ionic liquids, which are of great interest to the chemical and related industries because of their attractive properties as solvents, should be considered. Ionic liquids are comprised of an asymmetric, bulky organic cation and a weakly coordinating organic or inorganic anion. A large number of possible combinations allows for the ability to ‘fine tune’ the solvent properties for a specific purpose. Physical and chemical properties of ionic liquids are not only influenced by the nature of the cation and the nature of cation substituents but also by the polarity and the size of the anion. These features infer to ionic liquids numerous applications, in organic synthesis, separation processes, and electrochemistry. Separation processes required a good knowledge of the behavior of organic compounds with ionic liquids. Gas chromatography is a useful tool to estimate the interactions between organic compounds and ionic liquids. Indeed, retention data may be used to determine infinite dilution thermodynamic properties of volatile organic compounds in ionic liquids. Among others, the activity coefficient at infinite dilution is a direct measure of solute-ionic liquid interaction. In this work, infinite dilution thermodynamic properties of volatile organic compounds in specific bis(trifluoromethylsulfonyl)imide based ionic liquids measured by gas chromatography is presented. It was found that apolar compounds are not miscible in this family of ionic liquids. As expected, the solubility of organic compounds is related to their polarity and hydrogen-bond. Through activity coefficients data, the performance of these ionic liquids was evaluated for different separation processes (benzene/heptane, thiophene/heptane and pyridine/heptane). Results indicate that ionic liquids may be used for the extraction of polar compounds (aromatics, alcohols, pyridine, thiophene, tetrahydrofuran) from aliphatic media. For example, 1-benzylpyridinium bis(trifluoromethylsulfonyl) imide and 1-cyclohexylmethyl-1-methylpyrrolidinium bis(trifluoromethylsulfonyl)imide are more efficient for the extraction of aromatics or pyridine from aliphatics than classical solvents. Ionic liquids with long alkyl chain length present important capacity values but their selectivity values are low. In conclusion, we have demonstrated that specific bis(trifluoromethylsulfonyl)imide based ILs containing polar chain grafted on the cation (for example benzyl or cyclohexyl) increases considerably their performance in separation processes.

Keywords: interaction organic solvent-ionic liquid, gas chromatography, solvation model, COSMO-RS

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Authors: Sh. Najari Moghadam, M. Qomi, F. Raofie, J. Khadiv

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In this study, a liquid phase microextraction by hollow fiber (HF-LPME) combined with high performance liquid chromatography-UV detector was applied to preconcentrate and determine trace levels of Cyproheptadine in human urine and plasma samples. Cyproheptadine was extracted from 10 mL alkaline aqueous solution (pH: 9.81) into an organic solvent (n-octnol) which was immobilized in the wall pores of a hollow fiber. Then, it was back-extracted into an acidified aqueous solution (pH: 2.59) located inside the lumen of the hollow fiber. This method is simple, efficient and cost-effective. It is based on pH gradient and differences between two aqueous phases. In order to optimize the HF-LPME, some affecting parameters including the pH of donor and acceptor phases, the type of organic solvent, ionic strength, stirring rate, extraction time and temperature were studied and optimized. Under optimal conditions enrichment factor, limit of detection (LOD) and relative standard deviation (RSD(%), n=3) were up to 112, 15 μg.L−1 and 2.7, respectively.

Keywords: biological samples, cyproheptadine, hollow fiber, liquid phase microextraction

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Authors: Odunayo Christy Atewolara-Odule, Olapeju O. Aiyelaagbe

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The search for new natural anti-oxidants has grown tremendously over the years because reactive oxygen species (ROS) production and oxidative stress have been linked to a large number of human degenerative diseases, such as cancer, cardiovascular diseases, inflammation, and diabetes. Tapinanthus bangwensis, a parasitic plant commonly known as mistletoe belonging to the Loranthaceae family, is mostly employed traditionally to treat inflammation, cancer, diabetes, and hypertension to mention a few. In this study, air-dried pulverized leaves and stem of Tapinanthus bangwensis were successively extracted with n-hexane, ethyl acetate, and methanol to give the corresponding crude extracts. The extracts were purified by column chromatography and high-performance liquid chromatography to give the isolated compounds. Structural elucidation was done using mass spectrometry, Fourier transform infra-red, 1D and 2D NMR spectroscopy. The antioxidant activity of the compounds was evaluated using 2,2-diphenyl-1-picrylhydrazyl (DPPH) and ascorbic acid as standard. Three compounds; Friedelin, Eudesmic acid (3,4,5-trimethoxybenzoic) and Methyl-3,4,5-trimethoxybenzoate were isolated from the extracts of Tapinanthus bangwensis. Friedelin was isolated from the ethyl acetate extract of the stem while the two other compounds were isolated from the methanol extract of the leaves. The percentages of free radical scavenging activities of the compounds are as follows: Friedelin, 73.69%, methyl-3,4,5-trimethoxybenzoate, 79.33% and eudesmic, 87.68% anti-oxidant activity which were quite comparable to 93.96% given by ascorbic acid. We are reporting, to our best knowledge, for the first time the occurrence of friedelin and eudesmic acid in Tapinanthus bangwensis. The high anti-oxidant activity of these compounds supports the use of this plant in the management of diabetes and hypertension as they will be useful in combating complications arising from the disease.

Keywords: column chromatography, eudesmic acid, friedelin, Tapinanthus bangwensis

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Authors: Lidija R. Jevrić, Sanja O. Podunavac-Kuzmanović, Strahinja Z. Kovačević

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The present study deals with the selection of the most suitable quantitative structure-retention relationship (QSRR) models which should be used in prediction of the retention behavior of basic, neutral, acidic and phenolic pesticides which belong to different classes: fungicides, herbicides, metabolites, insecticides and plant growth regulators. Sum of ranking differences (SRD) approach can give a different point of view on selection of the most consistent QSRR model. SRD approach can be applied not only for ranking of the QSRR models, but also for detection of similarity or dissimilarity among them. Applying the SRD analysis, the most similar models can be found easily. In this study, selection of the best model was carried out on the basis of the reference ranking (“golden standard”) which was defined as the row average values of logarithm of retention time (logtr) defined by high performance liquid chromatography (HPLC). Also, SRD analysis based on experimental logtr values as reference ranking revealed similar grouping of the established QSRR models already obtained by hierarchical cluster analysis (HCA).

Keywords: chemometrics, chromatography, pesticides, sum of ranking differences

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Authors: Jana Andzane, Gunta Kunakova, Margarita Baitimirova, Mikelis Marnauza, Floriana Lombardi, Donats Erts

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Bismuth selenide (Bi₂Se₃) is known as a narrow band gap semiconductor with pronounced thermoelectric (TE) and topological insulator (TI) properties. Unique TI properties offer exciting possibilities for fundamental research as observing the exciton condensate and Majorana fermions, as well as practical application in spintronic and quantum information. In turn, TE properties of this material can be applied for wide range of thermoelectric applications, as well as for broadband photodetectors and near-infrared sensors. Nanostructuring of this material results in improvement of TI properties due to suppression of the bulk conductivity, and enhancement of TE properties because of increased phonon scattering at the nanoscale grains and interfaces. Regarding TE properties, crystallographic growth direction, as well as orientation of the nanostructures relative to the growth substrate, play significant role in improvement of TE performance of nanostructured material. For instance, Bi₂Se₃ layers consisting of randomly oriented nanostructures and/or of combination of them with planar nanostructures show significantly enhanced in comparison with bulk and only planar Bi₂Se₃ nanostructures TE properties. In this work, a catalyst-free vapour-solid deposition technique was applied for controlled obtaining of different types of Bi₂Se₃ nanostructures and continuous nanostructured layers for targeted applications. For example, separated Bi₂Se₃ nanoplates, nanobelts and nanowires can be used for investigations of TI properties; consisting from merged planar and/or randomly oriented nanostructures Bi₂Se₃ layers are useful for applications in heat-to-power conversion devices and infrared detectors. The vapour-solid deposition was carried out using quartz tube furnace (MTI Corp), equipped with an inert gas supply and pressure/temperature control system. Bi₂Se₃ nanostructures/nanostructured layers of desired type were obtained by adjustment of synthesis parameters (process temperature, deposition time, pressure, carrier gas flow) and selection of deposition substrate (glass, quartz, mica, indium-tin-oxide, graphene and carbon nanotubes). Morphology, structure and composition of obtained Bi₂Se₃ nanostructures and nanostructured layers were inspected using SEM, AFM, EDX and HRTEM techniques, as well as home-build experimental setup for thermoelectric measurements. It was found that introducing of temporary carrier gas flow into the process tube during the synthesis and deposition substrate choice significantly influence nanostructures formation mechanism. Electrical, thermoelectric, and topological insulator properties of different types of deposited Bi₂Se₃ nanostructures and nanostructured coatings are characterized as a function of thickness and discussed.

Keywords: bismuth seleinde, nanostructures, topological insulator, vapour-solid deposition

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Authors: D. S. Fardhyanti, A. Damayanti

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The utilization of biomass as a source of new and renewable energy is being carried out. One of the technologies to convert biomass as an energy source is pyrolysis which is converting biomass into more valuable products, such as bio-oil. Bio-oil is a liquid which is produced by steam condensation process from the pyrolysis of coconut shells. The composition of a coconut shell e.g. hemicellulose, cellulose and lignin will be oxidized to phenolic compounds as the main component of the bio-oil. The phenolic compounds in bio-oil are corrosive; they cause various difficulties in the combustion system because of a high viscosity, low calorific value, corrosiveness, and instability. Phenolic compounds are very valuable components which phenol has used as the main component for the manufacture of antiseptic, disinfectant (known as Lysol) and deodorizer. The experiments typically occurred at the atmospheric pressure in a pyrolysis reactor at temperatures ranging from 300 ^oC to 350 ^oC with a heating rate of 10 ^oC/min and a holding time of 1 hour at the pyrolysis temperature. The Gas Chromatography-Mass Spectroscopy (GC-MS) was used to analyze the bio-oil components. The obtained bio-oil has the viscosity of 1.46 cP, the density of 1.50 g/cm³, the calorific value of 16.9 MJ/kg, and the molecular weight of 1996.64. By GC-MS, the analysis of bio-oil showed that it contained phenol (40.01%), ethyl ester (37.60%), 2-methoxy-phenol (7.02%), furfural (5.45%), formic acid (4.02%), 1-hydroxy-2-butanone (3.89%), and 3-methyl-1,2-cyclopentanedione (2.01%).

Keywords: bio-oil, pyrolysis, coconut shell, phenol, gas chromatography-mass spectroscopy

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Authors: Anjana R. Menon, Anjana Bhasi

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Development of highways and railways play crucial role in a nation’s economic growth. While rigid concrete pavements are durable with high load bearing characteristics, growing economies mostly rely on flexible pavements which are easier in construction and more economical. The strength of flexible pavement is based on the strength of subgrade and load distribution characteristics of intermediate granular layers. In this scenario, to simultaneously meet economy and strength criteria, it is imperative to strengthen and stabilize the load transferring layers, namely subbase and base. Geosynthetic reinforcement in planar and cellular forms have been proven effective in improving soil stiffness and providing a stable load transfer platform. Studies have proven the relative superiority of cellular form-geocells over planar geosynthetic forms like geogrid, owing to the additional confinement of infill material and pocket effect arising from vertical deformation. Hence, the present study investigates the efficiency of geocells over single/multiple layer geogrid reinforcements by a series of three-dimensional model analyses of a flexible pavement section under a standard repetitive wheel load. The stress transfer mechanism and deformation profiles under various reinforcement configurations are also studied. Geocell reinforcement is observed to take up a higher proportion of stress caused by the traffic loads compared to single and double-layer geogrid reinforcements. The efficiency of single geogrid reinforcement reduces with an increase in embedment depth. The contribution of lower geogrid is insignificant in the case of the double-geogrid reinforced system.

Keywords: Geocell, Geogrid, Flexible Pavement, Repetitive Wheel Load, Numerical Analysis

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Authors: Tariq Ahmad Dar, Moinuddin, M. Masroor A. Khan

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There is considerable need in enhancing the content and yield of active constituents of medicinal plants keeping in view their massive demand worldwide. Different strategies have been employed to enhance the active constituents of medicinal plants and the use of phytohormones has been proved effective in this regard. Gamma-irradiated Sodium alginate (ISA) is known to elicit an array of plant defense responses and biological activities in plants. Considering the medicinal importance, a pot experiment was conducted to explore the effect of ISA and phosphorus on growth, yield and quality of fenugreek (Trigonella foenum-graecum L.). ISA spray treatments (0, 40, 80 and 120 mg L-1) were applied alone and in combination with 40 kg P ha-1 (P40). Crop performance was assessed in terms of plant growth characteristics, physiological attributes, seed yield and the content of seed trigonelline. Of the ten-treatments, P40 + 80 mg L−1 of ISA proved the best. The results showed that foliar spray of ISA alone or in combination with P40 augmented the plant vegetative growth, enzymatic activities, trigonelline content, trigonelline yield and economic yield of fenugreek. Application of 80 mg L−1 of ISA applied with P40 gave the best results for almost all the parameters studied compared to control or to 80 mg L−1 of ISA applied alone. This treatment increased the total content of chlorophyll, carotenoids, leaf -N, -P and -K and trigonelline compared to the control by 24.85 and 27.40%, 15 and 23.52%, 18.70 and 16.84%, 15.88 and 18.92%, 12 and 14.44%, at 60 and 90 DAS respectively. The combined application of 80 mg L−1 of ISA along with P40 resulted in the maximum increase in seed yield, trigonelline content and trigonelline yield by146, 34 and 232.41%, respectively, over the control. Gel permeation chromatography revealed the formation of low molecular weight fractions in ISA samples, containing even less than 20,000 molecular weight oligomers, which might be responsible for plant growth promotion in this study. Trigonelline content was determined by reverse phase high performance liquid chromatography (HPLC) with C-18 column.

Keywords: gamma-irradiated sodium alginate, phosphorus, gel permeation chromatography, HPLC, trigonelline content, yield

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Authors: Hye Rim Kang, So Yae Koh, Ji-Yeon Ryu, Chang Kyu Lee, Ji Hee Lim, Hyeon A. Kim, Geun Hyung Im, Somi Kim Cho

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In this study, antioxidant properties and compositional analysis of fermented chocolate were examined. Chocolate was fermented with Lactobacillus plantarum CK10. As fermentation time went by, pH was decreased (5.26±0.02 to 3.98±0.06) while titratable acidity was increased (5.36±0.19 to 13.31±0.34). The total polyphenol contents were maintained through the fermentation. The contents of total polyphenol were slightly increased at 8 hr (6.34±0.12 mg GAE (Gallic acid equivalent)/g), and it reached to comparable levels of the control at 24 hr (control, 5.47±0.36 mg GAE/g); 24 hr, 5.19±0.23 mg GAE/g). Similarly, the total flavonoid contents were not significantly changed during fermentation. The pronounced radical scavenging activities of chocolate, against DPPH-, ABTS-, and Alkyl radical, were observed. The levels of antioxidant activities were not dramatically altered in the course of fermentation. By gas chromatography-mass spectrometry analysis, the increase in lactic acid was measured and four major compounds, HMF, xanthosine, caffeine, and theobromine, were identified. The relative peak area of caffeine and theobromine was considerably changed during fermentation. However, no significant difference in the levels of caffeine and theobromine were observed by high-performance liquid chromatography analysis.

Keywords: antioxidant, chocolate, compositional analysis, fermentation, Lactobaillus plantarum

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