Search results for: gas chromatography jojoba esters

Authors: Ishan Arora, Anurag Rathore

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The primary objective of this work was to study the effect of resin chemistry, pH and molarity of binding and elution buffer on aggregate removal using Cation Exchange Chromatography and find the optimum conditions which can give efficient aggregate removal with minimum loss of yield. Four different resins were used for carrying out the experiments: Fractogel EMD SO3-(S), Fractogel EMD COO-(M), Capto SP ImpRes and S Ceramic HyperD. Runs were carried out on the AKTA Avant system. Design of Experiments (DOE) was used for analysis using the JMP software. The dependence of the yield obtained using different resins on the operating conditions was studied. Success has been achieved in obtaining yield greater than 90% using Capto SP ImpRes and Fractogel EMD COO-(M) resins. It has also been found that a change in the operating conditions generally has different effects on the yields obtained using different resins.

Keywords: aggregates, cation exchange chromatography, design of experiments, monoclonal antibodies

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Authors: Jenson George, Thoa Nguyen, Garth Sanewski, Craig Hardner, Heather Eunice Smyth

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Pineapple (Ananas comosus), with its unique sweet flavour, is one of the most popular tropical, non-climacteric fruits consumed worldwide. It is also the third most important tropical fruit in world production. In Australia, 99% of the pineapple production is from the Queensland state due to the favourable subtropical climatic conditions. The flavourful fruit is known to contain around 500 volatile organic compounds (VOC) at varying concentrations and greatly contribute to the flavour quality of pineapple fruit by providing distinct aroma sensory properties that are sweet, fruity, tropical, pineapple-like, caramel-like, coconut-like, etc. The aroma of pineapple is one of the important factors attracting consumers and strengthening the marketplace. To better understand the aroma of Australian-grown pineapples, the matrix-matched Gas chromatography–mass spectrometry (GC-MS), Head Space - Solid-phase microextraction (HS-SPME), Stable-isotope dilution analysis (SIDA) method was developed and validated. The developed method represents a significant improvement over current methods with the incorporation of multiple external reference standards, multiple isotopes labeled internal standards, and a matching model system of pineapple fruit matrix. This method was employed to quantify 28 key aroma compounds in more than 200 genetically diverse pineapple varieties from a breeding program. The Australian pineapple cultivars varied in content and composition of free volatile compounds, which were predominantly comprised of esters, followed by terpenes, alcohols, aldehydes, and ketones. Using selected commercial cultivars grown in Australia, and by employing the sensorial analysis, the appearance (colour), aroma (intensity, sweet, vinegar/tang, tropical fruits, floral, coconut, green, metallic, vegetal, fresh, peppery, fermented, eggy/sulphurous) and texture (crunchiness, fibrousness, and juiciness) were obtained. Relationships between sensory descriptors and volatiles were explored by applying multivariate analysis (PCA) to the sensorial and chemical data. The key aroma compounds of pineapple exhibited a positive correlation with corresponding sensory properties. The sensory and volatile data were also used to explore genetic diversity in the breeding population. GWAS was employed to unravel the genetic control of the pineapple volatilome and its interplay with fruit sensory characteristics. This study enhances our understanding of pineapple aroma (flavour) compounds, their biosynthetic pathways and expands breeding option for pineapple cultivars. This research provides foundational knowledge to support breeding programs, post-harvest and target market studies, and efforts to optimise the flavour of commercial pineapple varieties and their parent lines to produce better tasting fruits for consumers.

Keywords: Ananas comosus, pineapple, flavour, volatile organic compounds, aroma, Gas chromatography–mass spectrometry (GC-MS), Head Space - Solid-phase microextraction (HS-SPME), Stable-isotope dilution analysis (SIDA).

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Authors: Xiang Li, Kui Chen, Bin Wu, Min Zhou

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Sclareolide is made from sclareol by oxidiative synthesis and subsequent crystallization, while the crystallization mother liquor still contains 15%~30%wt of sclareolide to be reclaimed. With the reaction material of sclareol is provided as plant extract, many sorts of complex impurities exist in the mother liquor. Due to the difficulty in recycling sclareolide after solvent recovery, it is common practice for the factories to discard the mother liquor, which not only results in loss of sclareolide, but also contributes extra environmental burden. In this paper, a process based on adsorption and elution has been presented for recycling of sclareolide from mother liquor. After pretreatment of the crystallization mother liquor by HZ-845 resin to remove parts of impurities, sclareolide is adsorbed by HZ-816 resin. The HZ-816 resin loaded with sclareolide is then eluted by elution solvent. Finally, the eluent containing sclareolide is concentrated and fed into the crystallization step in the process. By adoption of the recycle from mother liquor, total yield of sclareolide increases from 86% to 90% with a stable purity of the final sclareolide products maintained.

Keywords: sclareolide, resin, adsorption, chromatography

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Authors: Jelka Pleadin, Greta Krešić, Tina Lešić, Ana Vulić, Renata Barić, Tanja Bogdanović, Dražen Oraić, Ana Legac, Snježana Zrnčić

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Fish has been acknowledged as an integral component of a well-balanced diet, providing a healthy source of energy, high-quality proteins, vitamins, essential minerals and, especially, n-3 long-chain polyunsaturated fatty acids (n-3 LC PUFA), mainly eicosapentaenoic acid (20:5 n-3 EPA), and docosahexaenoicacid, (22:6 n-3 DHA), whose pleiotropic effects in terms of health promotion and disease prevention have been increasingly recognised. In this study, the fatty acids composition of three commercially important farmed fish species: sea bream (Sparus aurata), sea bass (Dicentrarchus labrax) and dentex (Dentex dentex) was investigated. In total, 60 fish samples were retrieved during 2015 (n = 30) and 2016 (n = 30) from different locations in the Adriatic Sea. Methyl esters of fatty acids were analysed using gas chromatography (GC) with flame ionization detection (FID). The results show that the most represented fatty acid in all three analysed species is oleic acid (C18:1n-9, OA), followed by linoleic acid (C18:2n-6, LA) and palmitic acid (C16:0, PA). Dentex was shown to have two to four times higher eicosapentaenoic (EPA) and docosahexaenoic (DHA) acid content as compared to sea bream and sea bass. The recommended n-6/n-3 ratio was determined in all fish species but obtained results pointed to statistically significant differences (p < 0.05) in fatty acid composition among the analysed fish species and their potential as a dietary source of valuable fatty acids. Sea bass and sea bream had a significantly higher proportion of n-6 fatty acids, while dentex had a significantly higher proportion of n-3 (C18:4n-3, C20:4n-3, EPA, DHA) fatty acids. A higher hypocholesterolaemic and hypercholesterolaemic fatty acids (HH) ratio was determined for sea bass and sea bream, which comes as the consequence of a lower share of SFA determined in these two species in comparison to dentex. Since the analysed fish species vary in their fatty acids composition consumption of diverse fish species would be advisable. Based on the established lipid quality indicators, dentex, a fish species underutilised by the aquaculture, seems to be a highly recommendable and important source of fatty acids recommended to be included into the human diet.

Keywords: dentex, fatty acids, farmed fish, sea bass, sea bream

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Authors: Alexandre Gonzalez, Zohra Benfodda, David Bénimélis, Jean-Xavier Fontaine, Roland Molinié, Patrick Meffre

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Volatile organic compounds (VOCs) emitted by flowers play an important role in plant ecology. However, the Tillandsia genus has been scarcely studied according to the VOCs emitted by flowers. Tillandsia are epiphytic flowering plants belonging to the Bromeliaceae family. The VOCs composition of twelve unscented and two faint-scented Tillandsia species was studied. The headspace solid phase microextraction coupled with gas chromatography combined with mass spectrometry method was used to explore the chemical diversity of the VOCs. This study allowed the identification of 65 VOCs among the fourteen species, and between six to twenty-five compounds were identified in each of the species.

Keywords: tillandsia, headspace solid phase microextraction (HS-SPME), gas chromatography-mass spectrometry (GC-MS), scentless flowers, volatile organic compounds (VOCs), PCA analysis, heatmap

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Authors: Layla El Gaini, Majdouline Belaqziz, Meriem Outaki, Mariam Minhaj

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In this study, it introduce and validate a high-performance liquid chromatography method with diode-array detection (HPLC-DAD) specifically designed for the accurate quantification of caffeic acid in phenolic extracts obtained from olive mill wastewater. The separation process of caffeic acid was effectively achieved through the use of an Acclaim Polar Advantage column (5µm, 250x4.6mm). A meticulous multi-step gradient mobile phase was employed, comprising water acidified with phosphoric acid (pH 2.3) and acetonitrile, to ensure optimal separation. The diode-array detection was adeptly conducted within the UV–VIS spectrum, spanning a range of 200–800 nm, which facilitated precise analytical results. The method underwent comprehensive validation, addressing several essential analytical parameters, including specificity, repeatability, linearity, as well as the limits of detection and quantification, alongside measurement uncertainty. The generated linear standard curves displayed high correlation coefficients, underscoring the method's efficacy and consistency. This validated approach is not only robust but also demonstrates exceptional reliability for the focused analysis of caffeic acid within the intricate matrices of wastewater, thus offering significant potential for applications in environmental and analytical chemistry.

Keywords: high-performance liquid chromatography (HPLC-DAD), caffeic acid analysis, olive mill wastewater phenolics, analytical method validation

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Authors: Vijayalakshmi Marella, NageswaraRaoPilli

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This paper describes a simple, rapid and sensitive liquid chromatography / tandem mass spectrometry assay for the determination of montelukast in human plasma using montelukast d6 as an internal standard. Analyte and the internal standard were extracted from 50 µL of human plasma via solid phase extraction technique without evaporation, drying and reconstitution steps. The chromatographic separation was achieved on a C18 column by using a mixture of methanol and 5mM ammonium acetate (80:20, v/v) as the mobile phase at a flow rate of 0.8 mL/min. Good linearity results were obtained during the entire course of validation. Method validation was performed as per FDA guidelines and the results met the acceptance criteria. A run time of 2.5 min for each sample made it possible to analyze more number of samples in short time, thus increasing the productivity. The proposed method was found to be applicable to clinical studies.

Keywords: Montelukast, tandem mass spectrometry, montelukast d6, FDA guidelines

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Authors: Suhaila Qari, Samia Moharram, Safaa Alowaidi

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Objectives: To determine the fatty acids profiles in female fish, R. sarba from the Red Sea during the spawning season. Methods: Monthly individual Rhabdosargus sarba were obtained from Bangalah market in Jeddah, Red Sea and transported to the laboratory in ice aquarium. The total length, standard length and weight were measured, fishes were dissected. Ovaries were removed, weighed and 10 ml of concentrated hydrochloric acid were added to 10g of the ovary in a conical flask and immersed in boiling water until the sample was dissolved and the fat was seen to collect on the surface. The conical was cooled and the fat was extracted by shaking with 30 ml of diethyl ether. The extract was bowled after allowing the layers to separate into a weighed flask. The extraction was repeated three times more and distilled off the solvent then the fat dried at 100oC, cooled and weighed. Then 50 mg of lipid was put in a tube, 5 ml of methanolic sulphuric acid was added and 2 ml of benzene, the tube well closed and placed in water bath at 90oC for an hour and half. After cooling, 8 ml water and 5 ml petroleum was added shacked strongly and the ethereal layer was separated in a dry tube, evaporated to dryness. The fatty acid methyl esters were analyzed using a Hewlett Packard (HP 6890) chromatography, asplit /splitless injector and flame ionization detector (FID). Results: In female Rhabdosargus sarba, a total of 29 fatty acids detected in ovaries throughout the spawning season. The main fatty acid group in total lipid was saturated fatty acid (SFA, 28.9%), followed by 23.5% of polyunsaturated fatty acids (PUFA) and 12.9% of monounsaturated fatty acids (MUFA). The dominant SFA were palmitic and stearic, the major MUFA were palmitoleic and oleic, and the major PUFA were C18:2 and C22:2. During spawning stages no significant differences in total SFA, MUFA and PUFA, the highest value of SFA was in late spawning (36.78%). However, the highest value of MUFA and PUFA was in spawning (16.70% and 24.96% respectively). During spawning season there were a significant differences in total SFA between March (late spawning stage) and December (nearly ripe stage), (P < 0.05).

Keywords: sparidae, Rhabdosargus sarba, fish, fatty acids, spawning, gonads, red sea

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Authors: Naureen Akhtar

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The stability of the protein in detergent-containing solution is the key for its successful crystallisation. Fluorescence-detection size-exclusion chromatography (FSEC) is a potential approach for screening monodispersity as well as the stability of protein in a detergent-containing-solution. In this present study, covalently linked Green Fluorescent Protein (GFP) to bacterial nitrate transporter, NarU from Escherichia coli was studied for pre-crystallisation trials by FSEC. Immobilised metal ion affinity chromatography (IMAC) and gel filtration were employed for their purification. The main objectives of this study were over-expression, detergent screening and crystallisation of nitrate transporter proteins. This study could not produce enough proteins that could realistically be taken forward to achieve the objectives set for this particular research. In future work, different combinations of variables like vectors, tags, creation of mutant proteins, host cells, position of GFP (N- or C-terminal) and/or membrane proteins would be tried to determine the best combination as the principle of technique is still promising.

Keywords: transporters, detergents, over-expression, crystallography

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Authors: Christiana Ene Ogwuche, Joseph Amupitan, George Ndukwe, Rachael Ayo

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Maesobotrya barteri (Baill), belonging to the family Euphorbiaceae, is a medicinal plant growing widely in tropical Africa. The Aerial plant parts of Maesobotrya barteri (Baill) were collected fresh from Orokam, Ogbadibo local Government of Benue State, Nigeria in July 2013. Taxonomical identification was done by Mallam Musa Abdullahi at the Herbarium unit of Biological Sciences Department, ABU, Zaria, Nigeria. Pulverized aerial parts of Maesobotrya barteri (960g) was exhaustively extracted successively using petroleum ether, chloroform, ethyl acetate and methanol and concentrated in the rotary evaporator at 40°C. The Petroleum ether extract had the second highest activity against test microbes from preliminary crude microbial screenings. The Petroleum ether extract was subjected to phytochemical studies, antimicrobial analysis and column chromatography (CC). The column chromatography yielded fraction PE, which was further purified using preparative thin layer chromatography to give PE1. The structure of the isolated compound was established using 1-D NMR and 2-D NMR spectroscopic analysis and by direct comparison with data reported in literature was confirmed to be a mixture, an isomer of Betulinic acid and Oleanolic acid, both with the molecular weight (C₃₀H₄₈O₃). The bioactivity of this compound was carried out using some clinical pathogens and the activity compared with standard drugs, and this was found to be comparable with the standard drug.

Keywords: Maesobotrya barteri, medicinal plant, bioactivity, petroleum spirit extract, butellinic acid, oleanilic acid

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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: Mohan H., C. Elajchet Senni

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In the present of high energy consumption in every sphere of life, renewable energy sources are emerging as alternative to conventional fuels for energy security, mitigating green house gas emission and climate change. There has been a world wide interest in searching for alternatives to petroleum derived fuels due to their depletion as well as due to the concern for the environment. Vegetable oils have capability to solve this problem because they are renewable and lead to reduction in environmental pollution. But high smoke emission and lower thermal efficiency are the main problems associated with the use of neat vegetable oils in diesel engines. In the present work, performance, combustion and emission characteristics of CI engine fuelled with 20% by vol. methyl esters mixed with Karanja seed Oil, and Fuel injection pressures of 200 bar and 240 bar, injection timings (21°,23° and 25° BTDC) and Proportion B20 diesel respectively. Vegetable oils have capability to solve this problem because they are renewable and lead to reduction in environmental pollution. But, high smoke emission and lower thermal efficiency are the main problems associated with the use of neat vegetable oils in diesel engines. In the present work, performance, combustion and emission characteristics of CI engine fuelled with 20% by vol. methyl esters mixed with Karanja seed Oil, and Fuel injection pressures of 200 bar and 240 bar ,Injection timings (21°,23° and 25° BTDC) and Proportion B20 diesel respectively. Various performance, combustion and emission characteristics such as thermal efficiency, and brake specific fuel consumption, maximum cylinder pressure, instantaneous heat release, cumulative heat release with respect to crank angle, ignition lag, combustion duration, HC, NOx, CO, exhaust temperature and smoke intensity were measured.

Keywords: karanja oil, injection pressure, injection timing, karanja oil methyl ester

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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: N. Chougui, R. Larbat

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The first economic importance of Opuntia ficus-indica relies on the production of edible fruits. This food transformation generates a large amount of by-products (seeds and peels) in addition to cladodes produced by the plant. Several studies showed the richness of these products with bioactive substances like phenolics that have potential applications. Indeed, phenolics have been associated with protection against oxidation and several biological activities responsible of different pathologies. Consequently, there has been a growing interest in identifying natural antioxidants from plants. This study falls within the framework of the industrial exploitation of by-products of the plant. The study aims to investigate the metabolic profile of three by-products (cladodes, peel seeds) regarding total phenolic content by liquid chromatography coupled to mass spectrometry approach (LC-MSn). The byproducts were first washed, crushed and stored at negative temperature. The total phenolic compounds were then extracted by aqueous-ethanolic solvent in order to be quantified and characterized by LC-MS. According to the results obtained, the peel extract was the richest in phenolic compounds (1512.58 mg GAE/100 g DM) followed by the cladode extract (629.23 GAE/100 g DM) and finally by the seed extract (88.82 GAE/100 g DM) which is mainly used for its oil. The LC-MS analysis revealed diversity in phenolics in the three extracts and allowed the identification of hydroxybenzoic acids, hydroxycinnamic acids and flavonoids. The highest complexity was observed in the seed phenolic composition; more than twenty compounds were detected that belong to acids esters among which three feruloyl sucrose isomers. Sixteen compounds belonging to hydroxybenzoic acids, hydroxycinnamic acids and flavonoids were identified in the peel extract, whereas, only nine compounds were found in the cladode extract. It is interesting to highlight that the phenolic composition of the cladode extract was closer to that of the peel exact. However, from a quantitative viewpoint, the peel extract presented the highest amounts. Piscidic and eucomic acids were the two most concentrated molecules, corresponding to 271.3 and 121.6 mg GAE/ 100g DM respectively. The identified compounds were known to have high antioxidant and antiradical potential with the ability to inhibit lipid peroxidation and to exhibit a wide range of biological and therapeutic properties. The findings highlight the importance of using the Opuntia ficus-indica by-products.

Keywords: characterization, LC-MSn analysis, Opuntia ficus-indica, phenolics

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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: Thummalapalli CSM Gupta, Banti Sidhiwala

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Mineral oils of naphthenic and paraffinic type have been traditionally been used as insulating liquids in the transformer applications to protect the solid insulation from moisture and ensures effective heat transfer/cooling. The performance of these type of oils have been proven in the field over many decades and the condition monitoring and diagnosis of transformer performance have been successfully monitored through oil properties and dissolved gas analysis methods successfully. Different type of gases representing various types of faults due to components or operating conditions effectively. While large amount of data base has been generated in the industry on dissolved gas analysis for mineral oil based transformer oils and various models for predicting the fault and analysis, oil specifications and standards have also been modified to include stray gassing limits which cover the low temperature faults and becomes an effective preventative maintenance tool that can benefit greatly to know the reasons for the breakdown of electrical insulating materials and related components. Natural esters have seen a rise in popularity in recent years due to their "green" credentials. Some of its benefits include biodegradability, a higher fire point, improvement in load capability of transformer and improved solid insulation life than mineral oils. However, the Stray gases evolution like hydrogen and hydrocarbons like methane (CH4) and ethane (C2H6) show very high values which are much higher than the limits of mineral oil standards. Though the standards for these type esters are yet to be evolved, the higher values of hydrocarbon gases that are available in the market is of concern which might be interpreted as a fault in transformer operation. The current paper focuses on developing a natural ester based transformer oil which shows very levels of stray gassing by standard test methods show much lower values compared to the products available currently and experimental results on various test conditions and the underlying mechanism explained.

Keywords: biodegadability, fire point, dissolved gassing analysis, stray gassing

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Authors: F. Murilo T. Luna, Vanessa F. Oliveira, Alysson Rocha, Expedito J. S. Parente, Andre V. Bueno, Matheus C. M. Farias, Celio L. Cavalcante Jr.

Abstract:

Aviation jetfuel used in aircraft gas-turbine engines is customarily obtained from the kerosene distillation fraction of petroleum (150-275°C). Mineral jetfuel consists of a hydrocarbon mixture containing paraffins, naphthenes and aromatics, with low olefins content. In order to ensure their safety, several stringent requirements must be met by jetfuels, such as: high energy density, low risk of explosion, physicochemical stability and low pour point. In this context, aviation fuels eventually obtained from biofeedstocks (which have been coined as ‘biojetfuel’), must be used as ‘drop in’, since adaptations in aircraft engines are not desirable, to avoid problems with their operation reliability. Thus, potential aviation biofuels must present the same composition and physicochemical properties of conventional jetfuel. Among the potential feedtstocks for aviation biofuel, the babaçu oil, extracted from a palm tree extensively found in some regions of Brazil, contains expressive quantities of short chain saturated fatty acids and may be an interesting choice for biojetfuel production. In this study, biojetfuel was synthesized through homogeneous transesterification of babaçu oil using methanol and its properties were compared with petroleum-based jetfuel through measurements of oxidative stability, physicochemical properties and low temperature properties. The transesterification reactions were carried out using methanol and after decantation/wash procedures, the methyl esters were purified by molecular distillation under high vacuum at different temperatures. The results indicate significant improvement in oxidative stability and pour point of the products when compared to the fresh oil. After optimization of operational conditions, potential biojetfuel samples were obtained, consisting mainly of C8 esters, showing low pour point and high oxidative stability. Jet engine tests are being conducted in an automated test bed equipped with pollutant emissions analysers to study the operational performance of the biojetfuel that was obtained and compare with a mineral commercial jetfuel.

Keywords: biojetfuel, babaçu oil, oxidative stability, engine tests

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

Abstract:

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: Rajeshkumar Kanubhai Patel, Neha Sudhirkumar Mochi

Abstract:

A simple and accurate stability-indicating, reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for the simultaneous quantitation of Evogliptin tartrate and Metformin HCl in pharmaceutical dosage forms, following ICH guidelines. Forced degradation was performed under various stress conditions including acid, base, oxidation, thermal, and photodegradation. The method utilized an Eclipse C18 column (250 mm × 4.6 mm, 5 µm) with a mobile phase of 5 mM 1-hexane sulfonic acid sodium salt in water and 0.2% v/v TEA (45:55 %v/v), adjusted to pH 3.0 with OPA, at a flow rate of 1.0 mL/min. Detection at 254.4 nm using a PDA detector showed good resolution of degradation products and both drugs. Linearity was observed within 1-5 µg/mL for Evogliptin tartrate and 100-500 µg/mL for Metformin HCl, with % recovery between 99-100% and precision within acceptable limits (%RSD < 2%). The method proved to be specific, precise, accurate, and robust for routine analysis of these drugs.

Keywords: stability indicating RP-HPLC, evogliptin tartrate, metformin HCl, validation

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Authors: Birute Bugelyte, Ingrida Jurkute, Vida Vickackaite

Abstract:

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

Abstract:

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

Abstract:

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

Abstract:

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

Abstract:

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

Procedia PDF Downloads 391