Search results for: method of gas chromatography

Authors: Hoda Mahgoub, Abeer Hanafy

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Linagliptin (LNG) belongs to dipeptidyl-peptidase-4 (DPP-4) inhibitor class. DPP-4 inhibitors represent a new therapeutic approach for the treatment of type 2 diabetes in adults. The aim of this work was to develop and validate an accurate and reproducible HPLC method for the determination of LNG with high sensitivity in rat plasma. The method involved separation of both LNG and pindolol (internal standard) at ambient temperature on a Zorbax Eclipse XDB C18 column and a mobile phase composed of 75% methanol: 25% formic acid 0.1% pH 4.1 at a flow rate of 1.0 mL.min-1. UV detection was performed at 254nm. The method was validated in compliance with ICH guidelines and found to be linear in the range of 5–1000ng.mL-1. The limit of quantification (LOQ) was found to be 5ng.mL-1 based on 100µL of plasma. The variations for intra- and inter-assay precision were less than 10%, and the accuracy values were ranged between 93.3% and 102.5%. The extraction recovery (R%) was more than 83%. The method involved a single extraction step of a very small plasma volume (100µL). The assay was successfully applied to an in-vivo pharmacokinetic study of LNG in rats that were administered a single oral dose of 10mg.kg-1 LNG. The maximum concentration (Cmax) was found to be 927.5 ± 23.9ng.mL-1. The area under the plasma concentration-time curve (AUC0-72) was 18285.02 ± 605.76h.ng.mL-1. In conclusion, the good accuracy and low LOQ of the bioanalytical HPLC method were suitable for monitoring the full pharmacokinetic profile of LNG in rats. The main advantages of the method were the sensitivity, small sample volume, single-step extraction procedure and the short time of analysis.

Keywords: HPLC, linagliptin, pharmacokinetic study, rat plasma

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Authors: Bernadett Henn, Katalin Tálos, Éva Kováss Széles

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During the last 50 years, the worldwide permeation of the nuclear techniques induces several new problems in the environmental and in the human life. Nowadays, due to the increasing of the risk of terrorism worldwide, the potential occurrence of terrorist attacks using also weapon of mass destruction containing radioactive or nuclear materials as e.g. dirty bombs, is a real threat. For instance, the uranium pellets are one of the potential nuclear materials which are suitable for making special weapons. The nuclear forensics mainly focuses on the determination of the origin of the confiscated or found nuclear and other radioactive materials, which could be used for making any radioactive dispersive device. One of the most important signatures in nuclear forensics to find the origin of the material is the determination of the rare earth element patterns (REE) in the seized or found radioactive or nuclear samples. The concentration and the normalized pattern of the REE can be used as an evidence of uranium origin. The REE are the fourteen Lanthanides in addition scandium and yttrium what are mostly found together and really low concentration in uranium pellets. The problems of the REE determination using ICP-MS technique are the uranium matrix (high concentration of uranium) and the interferences among Lanthanides. In this work, our aim was to develop an effective chemical sample preparation process using extraction chromatography for separation the uranium matrix and the rare earth elements from each other following some publications can be found in the literature and modified them. Secondly, our purpose was the optimization of the ICP-MS measuring process for REE concentration. During method development, in the first step, a REE model solution was used in two different types of extraction chromatographic resins (LN® and TRU®) and different acidic media for environmental testing the Lanthanides separation. Uranium matrix was added to the model solution and was proved in the same conditions. Methods were tested and validated using REE UOC (uranium ore concentrate) reference materials. Samples were analyzed by sector field mass spectrometer (ICP-SFMS).

Keywords: extraction chromatography, nuclear forensics, rare earth elements, uranium

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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: Kooshan Nayebzadeh, Maryam Enteshari, Abdorreza Mohammadi

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The oxidative stability of mayonnaise under different storage temperatures (4 and 25˚C) during 6-month shelf-life was investigated by different analytical methods. In this study, headspace single-drop microextarction (HS-SDME) combined with gas chromatography-mass spectrometry (GC-MS) as a green, sensitive and rapid technique was applied to evaluate oxidative state in mayonnaise. Oxidation changes of extracted oil from mayonnaise were monitored by analytical parameters including peroxide value (PV), p-Anisidine value (p-An V), thiobarbituric acid value (TBA), and oxidative stability index (OSI). Hexanal and heptanal as secondary volatile oxidation compounds were determined by HS-SDME/GC-MS method in mayonnaise matrix. The rate of oxidation in mayonnaises increased during storage and it was determined greater at 25 ˚C. The values of Anisidine and TBA were gradually enhanced during 6 months, while the amount of OSI decreased. At both temperatures, the content of hexanal was higher than heptanal during all storage periods. Also significant increments in hexanal and heptanal concentrations in the second and sixth month of storage have been observed. Hexanal concentrations in mayonnaises which were stored at 25 ˚C and during storage time showed the highest values. It can be concluded that the temperature and duration of storage time are definitive parameters which affect on quality and oxidative stability of mayonnaise. Additionally, hexanal content in comparison to heptanal is a more reliable oxidative indicator and HS-SDME/GC-MS can be applied in a quick and simple manner.

Keywords: oxidative stability, mayonnaise, headspace single-drop microextarction (HS-SDME), shelf-life

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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: Soomal Hamza, Uzma Imran

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Organochlorine pesticides bio-accumulate into the fat of fish, birds, and animals through which it enters the human food cycle. Due to their persistence and stability in the environment, many health impacts are associated with them, most of which are carcinogenic in nature. In this study, the level of organochlorine pesticides has been detected in Keenjhar Lake and remediated using Rhizoremediation technique. 14 OC pesticides namely, Aldrin, Deldrin, Heptachlor, Heptachlor epoxide, Endrin, Endosulfun I and II, DDT, DDE, DDD, Alpha, Beta, Gamma BHC and two plants namely, Water Hyacinth and Slvinia Molesta were used in the system using pot experiment which processed for 11 days. A consortium was inoculated in both plants to increase its efficiency. Water samples were processed using liquide-liquid extraction. Sediments and roots samples were processed using Soxhlet method followed by clean-up and Gas Chromatography. Delta-BHC was the predominantly found in all samples with mean concentration (ppb) and standard deviation of 0.02 ± 0.14, 0.52 ± 0.68, 0.61 ± 0.06, in Water, Sediments and Roots samples respectively. The highest levels were of Endosulfan II in the samples of water, sediments and roots. Water Hyacinth proved to be better bioaccumulaor as compared to Silvinia Molesta. The pattern of compounds reduction rate by the end of experiment was Delta-BHC>DDD > Alpha-BHC > DDT> Heptachlor> H.Epoxide> Deldrin> Aldrin> Endrin> DDE> Endosulfun I > Endosulfun II. Not much significant difference was observed between the pots with the consortium and pots without the consortium addition. Phytoremediation is a promising technique, but more studies are required to assess the bioremediation potential of different aquatic plants and plant-endophyte relationship.

Keywords: aquatic plant, bio remediation, gas chromatography, liquid liquid extraction

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Authors: P. S. Jain, K. D. Bobade, S. J. Surana

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A simple, selective, precise and Stability-indicating High-performance thin-layer chromatographic method for analysis of Naftopidil both in a bulk and in pharmaceutical formulation has been developed and validated. The method employed, HPTLC aluminium plates precoated with silica gel as the stationary phase. The solvent system consisted of hexane: ethyl acetate: glacial acetic acid (4:4:2 v/v). The system was found to give compact spot for Naftopidil (Rf value of 0.43±0.02). Densitometric analysis of Naftopidil was carried out in the absorbance mode at 253 nm. The linear regression analysis data for the calibration plots showed good linear relationship with r2=0.999±0.0001 with respect to peak area in the concentration range 200-1200 ng per spot. The method was validated for precision, recovery and robustness. The limits of detection and quantification were 20.35 and 61.68 ng per spot, respectively. Naftopidil was subjected to acid and alkali hydrolysis, oxidation and thermal degradation. The drug undergoes degradation under acidic, basic, oxidation and thermal conditions. This indicates that the drug is susceptible to acid, base, oxidation and thermal conditions. The degraded product was well resolved from the pure drug with significantly different Rf value. Statistical analysis proves that the method is repeatable, selective and accurate for the estimation of investigated drug. The proposed developed HPTLC method can be applied for identification and quantitative determination of Naftopidil in bulk drug and pharmaceutical formulation.

Keywords: naftopidil, HPTLC, validation, stability, degradation

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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: Sudhanshu Sharma

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Lisinopril, 1-[N-{(s)-I-carboxy-3 phenyl propyl}-L-proline dehydrate is a lysine analog of enalaprilat, the active metabolite of enalapril. It is long-acting, non-sulhydryl angiotensin-converting enzyme (ACE) inhibitor that is used for the treatment of hypertension and congestive heart failure in daily dosage 10-80 mg. Pharmacological activity of lisinopril has been proved in various experimental and clinical studies. Owing to its importance and widespread use, efforts have been made towards the development of simple and reliable analytical methods. As per our literature survey, lisinopril in pharmaceutical formulations has been determined by various analytical methodologies like polaragraphy, potentiometry, and spectrophotometry, but most of these analytical methods are not too suitable for the Identification of lisinopril from clinical samples because of the interferences caused by the amino acids and amino groups containing metabolites present in biological samples. This report is an attempt in the direction of developing a simple and reliable method for on plate identification and quantification of lisinopril in pharmaceutical formulations as well as from human urine samples using silica gel H layers developed with a new mobile phase comprising of micellar solutions of N-cetyl-N, N, N-trimethylammonium bromide (CTAB). Micellar solutions have found numerous practical applications in many areas of separation science. Micellar liquid chromatography (MLC) has gained immense popularity and wider applicability due to operational simplicity, cost effectiveness, relatively non-toxicity and enhanced separation efficiency, low aggressiveness. Incorporation of aqueous micellar solutions as mobile phase was pioneered by Armstrong and Terrill as they accentuated the importance of TLC where simultaneous separation of ionic or non-ionic species in a variety of matrices is required. A peculiarity of the micellar mobile phases (MMPs) is that they have no macroscopic analogues, as a result the typical separations can be easily achieved by using MMPs than aqueous organic mobile phases. Previously MMPs were successfully employed in TLC based critical separations of aromatic hydrocarbons, nucleotides, vitamin K1 and K5, o-, m- and p- aminophenol, amino acids, separation of penicillins. The human urine analysis for identification of selected drugs and their metabolites has emerged as an important investigation tool in forensic drug analysis. Among all chromatographic methods available only thin layer chromatography (TLC) enables a simple fast and effective separation of the complex mixtures present in various biological samples and is recommended as an approved testing for forensic drug analysis by federal Law. TLC proved its applicability during successful separation of bio-active amines, carbohydrates, enzymes, porphyrins, and their precursors, alkaloid and drugs from urine samples.

Keywords: lisnopril, surfactant, chromatography, micellar solutions

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Authors: Candra Irawan, David Yudianto, Ahsanu Nadiyya, Dewi Anna Br Sitepu, Hanafi, Erna Styani

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Jelly drink was produced from a combination of both natural and synthetic materials, such as acesulfame potassium (acesulfame-K) as synthetic sweetener material. Acesulfame-K content in jelly drink could be determined by High-Performance Liquid Chromatography (HPLC), but this method needed validation due to having a change on the reagent addition step which skips the carrez addition and comparison of mix mobile phase (potassium dihydrogen phosphate and acetonitrile) with ratio from 75:25 to 90:10 to be more efficient and cheap. This study was conducted to evaluate the performance of determination method for acesulfame-K content in the jelly drink by HPLC. The method referred to Deutsches Institut fur Normung European Standard International Organization for Standardization (DIN EN ISO):12856 (1999) about Foodstuffs, Determination of acesulfame-K, aspartame and saccharin. The result of the correlation coefficient value (r) on the linearity test was 0.9987 at concentration range 5-100 mg/L. Detection limit value was 0.9153 ppm, while the quantitation limit value was 1.1932 ppm. The recovery (%) value on accuracy test for sample concentration by spiking 100 mg/L was 102-105%. Relative Standard Deviation (RSD) value for precision and homogenization tests were 2.815% and 4.978%, respectively. Meanwhile, the comparative and stability tests were tstat (0.136) < ttable (2.101) and |µ1-µ2| (1.502) ≤ 0.3×CV Horwitz. Obstinacy test value was tstat < ttable. It can be concluded that the HPLC  method for the determination of acesulfame-K in jelly drink product by HPLC has been valid and can be used for analysis with good performance.

Keywords: acesulfame-K, jelly drink, HPLC, validation

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Authors: Tanwarat Kajsongkram, Saowalux Rotamporn, Sirinat Limbunruang, Sirinan Thubthimthed.

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High-Performance Liquid Chromatography (HPLC) method was developed and validated for simultaneous estimation of 6-Gingerol(6G) and 6-Shogaol(6S) in joint pain relief gel containing ginger extract. The chromatographic separation was achieved by using C18 column, 150 x 4.6mm i.d., 5μ Luna, mobile phase containing acetonitrile and water (gradient elution). The flow rate was 1.0 ml/min and the absorbance was monitored at 282 nm. The proposed method was validated in terms of the analytical parameters such as specificity, accuracy, precision, linearity, range, limit of detection (LOD), limit of quantification (LOQ), and determined based on the International Conference on Harmonization (ICH) guidelines. The linearity ranges of 6G and 6S were obtained over 20-60 and 6-18 µg/ml respectively. Good linearity was observed over the above-mentioned range with linear regression equation Y= 11016x- 23778 for 6G and Y = 19276x-19604 for 6S (x is concentration of analytes in μg/ml and Y is peak area). The value of correlation coefficient was found to be 0.9994 for both markers. The limit of detection (LOD) and limit of quantification (LOQ) for 6G were 0.8567 and 2.8555 µg/ml and for 6S were 0.3672 and 1.2238 µg/ml respectively. The recovery range for 6G and 6S were found to be 91.57 to 102.36 % and 84.73 to 92.85 % for all three spiked levels. The RSD values from repeated extractions for 6G and 6S were 3.43 and 3.09% respectively. The validation of developed method on precision, accuracy, specificity, linearity, and range were also performed with well-accepted results.

Keywords: ginger, 6-gingerol, HPLC, 6-shogaol

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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: Al. Tsertsvadze. L. Ebralidze, I. Matchutadze. D. Berashvili, A. Bakuridze

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Peatlands are landscape elements, they are formed over a very long period by physical, chemical, biologic, and geologic processes. In the moderate zone of Caucasus, the Kolkheti lowlands are distinguished by the diversity of relictual plants, a high degree of endemism, orographic, climate, landscape, and other characteristics of high levels of biodiversity. The unique properties of the Kolkheti region lead to the formation of special, so-called, endemic peat peloids. The composition and properties of peloids strongly depend on peat-forming plants. Peat is considered a unique complex of raw materials, which can be used in different fields of the industry: agriculture, metallurgy, energy, biotechnology, chemical industry, health care. They are formed in permanent wetland areas. As a result of decay, higher plants remain in the anaerobic area, with the participation of microorganisms. Peat mass absorbs soil and groundwater. Peloids are predominantly rich with humic substances, which are characterized by high biological activity. Humic acids stimulate enzymatic activity, regenerative processes, and have anti-inflammatory activity. Objects of the research were Kolkheti peat peloids (Ispani, Anaklia, Churia, Chirukhi, Peranga) possessing different formation phases. Due to specific physical and chemical properties of research objects, the aim of the research was to develop analytical methods in order to study the chemical composition of the objects. The research was held using modern instrumental methods of analysis: Ultraviolet-visible spectroscopy and Infrared spectroscopy, Scanning Electron Microscopy, Centrifuge, dry oven, Ultraturax, pH meter, fluorescence spectrometer, Gas chromatography-mass spectrometry (GC-MS/MS), Gas chromatography. Based on the research ration between organic and inorganic substances, the spectrum of micro and macro elements, also the content of minerals was determined. The content of organic nitrogen was determined using the Kjeldahl method. The total composition of amino acids was studied by a spectrophotometric method using standard solutions of glutamic and aspartic acids. Fatty acid was determined using GC (Gas chromatography). Based on the obtained results, we can conclude that the method is valid to identify fatty acids in the research objects. The content of organic substances in the research objects was held using GC-MS. Using modern instrumental methods of analysis, the chemical composition of research objects was studied. Each research object is predominantly reached with a broad spectrum of organic (fatty acids, amino acids, carbocyclic and heterocyclic compounds, organic acids and their esters, steroids) and inorganic (micro and macro elements, minerals) substances. Modified methods used in the presented research may be utilized for the evaluation of cosmetological balneological and pharmaceutical means prepared on the base of Kolkheti's Sphagnum Peat Peloids.

Keywords: modern analytical methods, natural resources, peat, chemistry

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Authors: Ana Vulic, Tina Lesic, Nina Kudumija, Maja Kis, Manuela Zadravec, Nada Vahcic, Tomaz Polak, Jelka Pleadin

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Mycotoxins are toxic secondary metabolites produced by numerous types of molds. They can contaminate both food and feed so that they represent a serious public health concern. Production of dry-fermented meat products involves ripening, during which molds can overgrow the product surface, produce mycotoxins, and consequently contaminate the final product. Citrinin is a mycotoxin produced mainly by the Penicillium citrinum. Data on citrinin occurrence in both food and feed are limited. Therefore, there is a need for research on citrinin occurrence in these types of meat products. The LC-MS/MS method for citrinin determination was developed and validated. Sample preparation was performed using immunoaffinity columns, which resulted in clean sample extracts. Method validation included the determination of the limit of detection (LOD), the limit of quantification (LOQ), recovery, linearity, and matrix effect in accordance to the latest validation guidance. The determined LOD and LOQ were 0.60 µg/kg and 1.98 µg/kg, respectively, showing a good method sensitivity. The method was tested for its linearity in the calibration range of 1 µg/L to 10 µg/L. The recovery was 100.9 %, while the matrix effect was 0.7 %. This method was employed in the analysis of 47 samples of dry-fermented sausages collected from local households. Citrinin wasn’t detected in any of these samples, probably because of the short ripening period of the tested sausages that takes three months tops. The developed method shall be used to test other types of traditional dry-cured products, such as prosciuttos, whose surface is usually more heavily overgrown by surface molds due to the longer ripening period.

Keywords: citrinin, dry-fermented meat products, LC-MS/MS, mycotoxins

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Authors: Laure Wiest, Barbara Giroud, Azziz Assoumani, Francois Lestremau, Emmanuelle Vulliet

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Due to their production at high tonnages and their extensive use, surfactants are contaminants among those determined at the highest concentrations in wastewater. However, analytical methods and data regarding their occurrence in river water are scarce and concern only a few families, mainly anionic surfactants. The objective of this study was to develop an analytical method to extract and analyze a wide variety of surfactants in a minimum of steps, with a sensitivity compatible with the detection of ultra-traces in surface waters. 27 substances, from 12 families of surfactants, anionic, cationic and non-ionic were selected for method optimization. Different retention mechanisms for the extraction by solid phase extraction (SPE) were tested and compared in order to improve their detection by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). The best results were finally obtained with a C18 grafted silica LC column and a polymer cartridge with hydrophilic lipophilic balance (HLB), and the method developed allows the extraction of the three types of surfactants with satisfactory recoveries. The final analytical method comprised only one extraction and two LC injections. It was validated and applied for the quantification of surfactants in 36 river samples. The method's limits of quantification (LQ), intra- and inter-day precision and accuracy were evaluated, and good performances were obtained for the 27 substances. As these compounds have many areas of application, contaminations of instrument and method blanks were observed and considered for the determination of LQ. Nevertheless, with LQ between 15 and 485 ng/L, and accuracy of over 80%, this method was suitable for monitoring surfactants in surface waters. Application on French river samples revealed the presence of anionic, cationic and non-ionic surfactants with median concentrations ranging from 24 ng/L for octylphenol ethoxylates (OPEO) to 4.6 µg/L for linear alkylbenzenesulfonates (LAS). The analytical method developed in this work will therefore be useful for future monitoring of surfactants in waters. Moreover, this method, which shows good performances for anionic, non-ionic and cationic surfactants, may be easily adapted to other surfactants.

Keywords: anionic surfactant, cationic surfactant, LC-MS/MS, non-ionic surfactant, SPE, surface water

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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: Ravi Patel, Ravisinh Solanki, Dignesh Khunt

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A stability-indicating reverse phase high performance liquid chromatography (RP-HPLC) method was developed and validated for estimating Nirmatrelvir in its self-emulsifying drug delivery system (SEDDS). The separation of Nirmatrelvir and its degradation products was accomplished by employing an Agilent Zorbax Eclipse plus C18 (250 mm x 4.6 mm, 5 µm) column, through which the mobile phase 5 mM phosphate buffer (pH 4.0) as mobile phase A and Acetonitrile as mobile phase B in a ratio of (40:60 % v/v) was pumped at a flow rate of 1.0 mL/min, through the HPLC system. Chromatographic separation and elution were monitored by a photo-diode array detector at 210 nm. Stress studies have been employed to evaluate this method's ability to indicate stability. Nirmatrelvir was exposed to several stress conditions, such as acid, alkali, oxidative, photolytic, and thermal degradations. Significant degradation was observed during acid and alkali hydrolysis, and the resulting degradation product was successfully separated from the Nirmatrelvir peak, preventing any interference. Furthermore, the primary degradant produced under alkali degradation conditions was identified using UPLC-ESI-TQ-MS/MS. The method was validated in accordance with the International Council on Harmonization (ICH) and found to be selective, precise, accurate, linear, and robust. The apparent permeability of Nirmatrelvir SEDDS was 4.20 ± 0.21×10-6 cm/sec, and the average proportion of free drug recovered was 0.5%. The method developed in this study was feasible and accurate for routine quality control evaluation of Nirmatrelvir SEDDS.

Keywords: Nirmatrelvir, SEDDS, degradation study, HPLC, LC-MS/MS

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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: A. Mandić, M. Sakač, A. Mišan, B. Šojić, L. Petrović, I. Lončarević, B. Pajin, I. Sedej

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Aldehydes as secondary lipid oxidation products are highly specific to the oxidative degradation of particular polyunsaturated fatty acids present in foods. Gas chromatographic analysis of those volatile compounds has been widely used for monitoring of the deterioration of food products. Developed static headspace gas chromatography method using flame ionization detector (SHS GC FID) was applied to monitor the aldehydes present in processed foods such as bakery, meat and confectionary products. Five selected aldehydes were determined in samples without any sample preparation, except grinding for bakery and meat products. SHS–GC analysis allows the separation of propanal, pentanal, hexanal, heptanal and octanal, within 15min. Aldehydes were quantified in fresh and stored samples, and the obtained range of aldehydes in crackers was 1.62±0.05-9.95±0.05mg/kg, in sausages 6.62±0.46-39.16±0.39mg/kg; and in cocoa spread cream 0.48±0.01-1.13±0.02mg/kg. Referring to the obtained results, the following can be concluded, proposed method is suitable for different types of samples, content of aldehydes varies depending on the type of a sample, and differs in fresh and stored samples of the same type.

Keywords: lipid oxidation, aldehydes, crackers, sausage, cocoa cream spread

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Authors: K. Mohammed, M. Agarwal, J. Mewman, Y. Ren

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An optimum technic has been developed for extracting volatile organic compounds which contribute to the aroma of lime fruit (Citrus aurantifolia). The volatile organic compounds of healthy and infested lime fruit with California red scale Aonidiella aurantii were characterized using headspace solid phase microextraction (HS-SPME) combined with gas chromatography (GC) coupled flame ionization detection (FID) and gas chromatography with mass spectrometry (GC-MS) as a very simple, efficient and nondestructive extraction method. A three-phase 50/30 μm PDV/DVB/CAR fibre was used for the extraction process. The optimal sealing and fibre exposure time for volatiles reaching equilibrium from whole lime fruit in the headspace of the chamber was 16 and 4 hours respectively. 5 min was selected as desorption time of the three-phase fibre. Herbivorous activity induces indirect plant defenses, as the emission of herbivorous-induced plant volatiles (HIPVs), which could be used by natural enemies for host location. GC-MS analysis showed qualitative differences among volatiles emitted by infested and healthy lime fruit. The GC-MS analysis allowed the initial identification of 18 compounds, with similarities higher than 85%, in accordance with the NIST mass spectral library. One of these were increased by A. aurantii infestation, D-limonene, and three were decreased, Undecane, α-Farnesene and 7-epi-α-selinene. From an applied point of view, the application of the above-mentioned VOCs may help boost the efficiency of biocontrol programs and natural enemies’ production techniques.

Keywords: lime fruit, Citrus aurantifolia, California red scale, Aonidiella aurantii, VOCs, HS-SPME/GC-FID-MS

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Authors: Ozcan Baris Citil, Mehmet Akoz

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Effects of fatty acid composition and punicic acid contents of abdominal fat of Hy-line hens were investigated by the gas chromatographic method. Total 30 different fatty acids were determined in fatty acid compositions of eggs. These fatty acids were varied between C 8 to C 22. The punicic acid content of abdominal fats analysed was found to be higher percentages in the 90th day than those of 30th and 60th day. At the end of the experiment, total punicic acid contents of abdominal fats were significantly increased.

Keywords: fatty acids, gas chromatography, punicic acid, abdominal fats

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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: Jeong Woo Kang, MiYoung Baek, Ki-Suk Kim, Kwang-Jick Lee, ByungJae So

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Introduction: A fast, easy and sensitive detection method was developed and validated by liquid chromatography tandem mass spectrometry for the determination of marbofloxacin in pig plasma which was further applied to study the pharmacokinetics of marbofloxacin. Materials and Methods: The plasma sample (500 μL) was mixed with 1.5 ml of 0.1% formic acid in MeCN to precipitate plasma proteins. After shaking for 20 min, The mixture was centrifuged at 5,000 × g for 30 min. It was dried under a nitrogen flow at 50℃. 500 μL aliquot of the sample was injected into the LC-MS/MS system. Chromatographic analysis was carried out mobile phase gradient consisting 0.1% formic acid in D.W. (A) and 0.1% formic acid in MeCN (B) with C18 reverse phase column. Mass spectrometry was performed using the positive ion mode and the selected ion monitoring (MRM). Results and Conclusions: The method validation was performed in the sample matrix. Good linearities (R2>0.999) were observed and the quantified average recoveries of marbofloxacin were 87 - 92% at level of 10 ng g-1 -100 ng g-1. The percent of coefficient of variation (CV) for the described method was less than 10 % over the range of concentrations studied. The limits of detection (LOD) and quantification (LOQ) were 2 and 5 ng g-1, respectively. This method has also been applied successfully to pharmacokinetic analysis of marbofloxacin after intravenous (IV), intramuscular (IM) and oral administration (PO). The mean peak plasma concentration (Cmax) was 2,597 ng g-1at 0.25 h, 2,587 ng g-1at 0.44 h and 2,355 ng g-1at 1.58 h for IV, IM and PO, respectively. The area under the plasma concentration-time curve (AUC0–t) was 24.8, 29.0 and 25.2 h μg/mL for IV, IM and PO, respectively. The elimination half-life (T1/2) was 8.6, 13.1 and 9.5 for IV, IM and PO, respectively. Bioavailability (F) of the marbofloxacin in pig was 117 and 101 % for IM and PO, respectively. Based on these result, marbofloxacin does not have any obstacles as therapeutics to develop the oral formulations such as tablets and capsules.

Keywords: marbofloxacin, LC-MS/MS, pharmacokinetics, chromatographic

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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: 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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