Search results for: method of gas chromatography

Authors: Liping Qiu, Xiaofeng Zhang

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The ion chromatography method for the rapid determination of four anions (F⁻、Cl⁻、SO₄²⁻、NO₃⁻) in burial ground poles was optimized. The L₉(₃⁴) orthogonal test was used to determine the optimal parameters of sample pretreatment: accurately weigh 2.000g of sample, add 10mL of ultrapure water, and extract for 40min under the conditions of shaking temperature 40℃ and shaking speed 180 r·min-1. The eluent was 25 mmol/L KOH solution, the analytical column was Ion Pac® AS11-SH (250 mm × 4.0 mm), and the purified filtrate was measured by a conductivity detector. Under this method, the detection limit of each ion is 0.066～0.078mg/kg, the relative standard deviation is 0.86%～2.44% (n=7), and the recovery rate is 94.6～101.9.

Keywords: ion chromatography, tomb, anion (F⁻, Cl⁻, SO₄²⁻, NO₃⁻), environmental protection

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Authors: Jonida Canaj

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A simple method of extraction and determination of fifteen priority polycyclic aromatic hydrocarbons (PAHs) from drinking water using high performance liquid chromatography (HPLC) has been validated with limits of detection (LOD) and limits of quantification (LOQ), method recovery and reproducibility, and other factors. HPLC parameters, such as mobile phase composition and flow standardized for determination of PAHs using fluorescent detector (FLD). PAH was carried out by liquid-liquid extraction using dichloromethane. Linearity of calibration curves was good for all PAH (R², 0.9954-1.0000) in the concentration range 0.1-100 ppb. Analysis of standard spiked water samples resulted in good recoveries between 78.5-150%(0.1ppb) and 93.04-137.47% (10ppb). The estimated LOD and LOQ ranged between 0.0018-0.98 ppb. The method described has been used for determination of the fifteen PAHs contents in drinking water samples.

Keywords: high performance liquid chromatography, HPLC, method validation, polycyclic aromatic hydrocarbons, PAHs, water

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Authors: A. B. Bazaralieva, A. A. Turgumbayeva

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The phytosubstance from garlic was obtained by extraction with liquid carbon dioxide under critical conditions. Methods of processing raw materials are proposed, and the chemical composition of garlic is studied by gas chromatography and mass spectrometry. The garlic extract's composition was determined using gas chromatography (GC) and gas chromatography-mass spectrophotometry (GC-MS). The phytosubstance had 54 constituents. The extract included the following main compounds: Manool (39.56%), Viridifrolol (7%), Podocarpa-1,8,11,13-tetraen-3-one, 14-isopropyl-1,13-dimethoxy- 5,15 percent, (+)-2-Bornanone (4.29%), Thujone (3.49%), Linolic acid ethyl ester (3.41%), and 12-O-Methylcarn.

Keywords: Allium sativum, bioactive compounds of garlic, carbon dioxide extraction of garlic, GS-MS method

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Authors: Bazaraliyeva Aigerim Bakytzhanovna, Turgumbayeva Aknur Amanbekovna

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The phytosubstance from garlic was obtained by extraction with liquid carbon dioxide under critical conditions. Methods of processing raw materials are proposed, and the chemical composition of garlic is studied by gas chromatography and mass spectrometry. The garlic extract's composition was determined using gas chromatography (GC) and gas chromatography-mass spectrophotometry (GC-MS). The phytosubstance had 54 constituents. The extract included the following main compounds: Manool (39.56%), Viridifrolol (7%), Podocarpa-1,8,11,13-tetraen-3-one, 14-isopropyl-1,13-dimethoxy- 5,15 percent, (+)-2-Bornanone (4.29%), Thujone (3.49%), Linolic acid ethyl ester (3.41%), and 12-O-Methylcarn.

Keywords: allium sativum, bioactive compounds of garlic, carbon dioxide extraction of garlic, GS-MS method

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Authors: Pavel Shcherban, Vlad Golovanov

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Currently, there is an active geological exploration and development of the subsoil shelf of the Kaliningrad region. To carry out a comprehensive and accurate assessment of the volumes and degree of extraction of hydrocarbons from open deposits, it is necessary to establish not only a number of geological and lithological characteristics of the structures under study, but also to determine the oil quality, its viscosity, density, fractional composition as accurately as possible. In terms of considered works, gas chromatography is one of the most capacious methods that allow the rapid formation of a significant amount of initial data. The aspects of the application of the gas chromatography method for determining the chemical characteristics of the hydrocarbons of the Kaliningrad shelf fields are observed in the article, as well as the correlation-regression analysis of these parameters in comparison with the previously obtained chemical characteristics of hydrocarbon deposits located on the land of the region. In the process of research, a number of methods of mathematical statistics and computer processing of large data sets have been applied, which makes it possible to evaluate the identity of the deposits, to specify the amount of reserves and to make a number of assumptions about the genesis of the hydrocarbons under analysis.

Keywords: computer processing of large databases, correlation-regression analysis, hydrocarbon deposits, method of gas chromatography

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Authors: Fangyan Li, Lin Min Lee, Hui Zhu Peh, Shoet Harn Chan

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Advantame, a derivative of aspartame, is the latest addition to a family of low caloric and high potent dipeptide sweeteners which include aspartame, neotame and alitame. The use of advantame as a high-intensity sweetener in food was first accepted by Food Standards Australia New Zealand in 2011 and subsequently by US and EU food authorities in 2014, with the results from toxicity and exposure studies showing advantame poses no safety concern to the public at regulated levels. To our knowledge, currently there is barely any detailed information on the analytical method of advantame in food matrix, except for one report published in Japanese, stating a high performance liquid chromatography (HPLC) and liquid chromatography/ mass spectrometry (LC-MS) method with a detection limit at ppm level. However, the use of acid in sample preparation and instrumental analysis in the report raised doubt over the reliability of the method, as there is indication that stability of advantame is compromised under acidic conditions. Besides, the method may not be suitable for analyzing food matrices containing advantame at low ppm or sub-ppm level. In this presentation, a simple, specific and sensitive method for the determination of advantame in food is described. The method involved extraction with water and clean-up via solid phase extraction (SPE) followed by detection using liquid chromatography tandem mass spectrometry (LC-MS/MS) in negative electrospray ionization mode. No acid was used in the entire procedure. Single laboratory validation of the method was performed in terms of linearity, precision and accuracy. A low detection limit at ppb level was achieved. Satisfactory recoveries were obtained using spiked samples at three different concentration levels. This validated method could be used in the routine inspection of the advantame level in food.

Keywords: advantame, food, LC-MS/MS, sweetener

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Authors: Renata L. C. Leão, João E. Nascimento, Natalia C. E. S. Nascimento, Elaine S. Vasconcelos, Mércia L. Oliveira

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The quality control procedures of a radiopharmaceutical include the assessment of its chemical purity. The method suggested by international pharmacopeias consists of a thin layer chromatographic run. In this paper, the method proposed by the United States Pharmacopeia (USP) is compared to a direct method to determine the final concentration of aminopolyether in Fludeoxyglucose (¹⁸F-FDG) preparations. The approach (no chromatographic run) was achieved by placing the thin-layer chromatography (TLC) plate directly on an iodine vapor chamber. Both methods were validated and they showed adequate results to determine the concentration of aminopolyether in ¹⁸F-FDG preparations. However, the direct method is more sensitive, faster and simpler when compared to the reference method (with chromatographic run), and it may be chosen for use in routine quality control of ¹⁸F-FDG.

Keywords: chemical purity, Kryptofix 222, thin layer chromatography, validation

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Authors: M. O. Ezegbogu, H. B. Osadolor

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Lipsticks constitute a significant source of transfer evidence, and can, therefore, provide corroborative or inclusionary evidence in criminal investigation. This study aimed to determine the uniqueness and persistence of different lipstick smears using Thin Layer Chromatography (TLC), and Gas Chromatography with a Flame Ionisation Detector (GC-FID). In this study, we analysed lipstick smears retrieved from tea cups exposed to the environment for up to four weeks. The n-alkane content of each sample was determined using GC-FID, while TLC was used to determine the number of bands, and retention factor of each band per smear. This study shows that TLC gives more consistent results over a 4-week period than GC-FID. It also proposes a maximum exposure time of two weeks for the analysis of lipsticks left in the open using GC-FID. Finally, we conclude that neither TLC nor GC-FID can distinguish lipstick evidence recovered from hypothetical crime scenes.

Keywords: forensic science, chromatography, identification, lipstick

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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: Ahmed Aboforn

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Butene-1 product is consider effectively raw material in Polyethylene production, however Oxygenates impurities existing will be effected ethylene/butene-1 copolymers synthesized through titanium-magnesium-supported Ziegler-Natta catalysts. Laterally, Petrochemical industries are challenge against poor quality of Butene-1 and other C4 mix – feedstock that reflected on business impact and production losing. In addition, propylene product suffering from contamination by oxygenates components and causing for lose production and plant upset of Polypropylene process plants. However, Multidimensional gas chromatography (MDGC) innovative analytical methodology is a chromatography technique used to separate complex samples, as mixing different functional group as Hydrocarbon and oxygenates compounds and have similar retention factors, by running the eluent through two or more columns instead of the customary single column. This analytical study striving to enhance the quality of Oxygenates analytical method, as monitoring the concentration of oxygenates with accurate and precise analytical method by utilizing multidimensional GC supported by Backflush technique and Flame Ionization Detector, which have high performance separation of hydrocarbon and Oxygenates; also improving the minimum detection limits (MDL) to detect the concentration <1.0 ppm. However different types of oxygenates as (Alcohols, Aldehyde, Ketones, Ester and Ether) may be determined in other Hydrocarbon streams asC3, C4-mix, until C12 mixture, supported by liquid injection auto-sampler.

Keywords: analytical chemistry, gas chromatography, petrochemicals, oxygenates

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Authors: Totik Sri Mariani, Sukrasno Isna, Tet Fatt Chia

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Purwoceng (Pimpinella pruatjan Molk) is a legend plant used for increasing stamina by Kings in Java Island, Indonesia. Purpose of this study was to perform meristem culture and detected its stigmasterol by thin layer chromatography (TLC). Our result show that meristem culture could be propagated and grew into plantlet. After extracting intact acclimatized plant derived from meristem culture by hexane, we could detected stigmasterol by TLC. For suggestion, our extraction and TLC method could be used for detecting stigmasterol in others plant.

Keywords: purwoceng (pimpinella pruatjan), meristem culture, extraction, thin layer chromatography

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Authors: Ramandeep Kaur, Ashok Kumar Malik

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Fabric Phase Sorptive Extraction (FPSE) combined with Gas chromatography Mass Spectrometry (GCMS) has been developed for the determination of nineteen organochlorine pesticides in various aqueous samples. The method consolidates the features of sol-gel derived microextraction sorbents with rich surface chemistry of cellulose fabric substrate which could directly extract sample from complex sample matrices and incredibly improve the operation with decreased pretreatment time. Some vital parameters such as kind and volume of extraction solvent and extraction time were examinedand optimized. Calibration curves were obtained in the concentration range 0.5-500 ng/mL. Under the optimum conditions, the limits of detection (LODs) were in the range 0.033 ng/mL to 0.136 ng/mL. The relative standard deviations (RSDs) for extraction of 10 ng/mL 0f OCPs were less than 10%. The developed method has been applied for the quantification of these compounds in aqueous and fruit juice samples. The results obtained proved the present method to be rapid and feasible for the determination of organochlorine pesticides in aqueous samples.

Keywords: fabric phase sorptive extraction, gas chromatography-mass spectrometry, organochlorine pesticides, sample pretreatment

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Authors: Nadeem A. Siddique, Mohd Mujeeb, Kahkashan

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Introduction: The objective of the projected work is to study the occurrence of the aflatoxins B1, B2, G1and G2 in remedial plants, exclusively in Delphinium denudatum. The aflatoxins were analysed by high-performance liquid chromatography–tandem quadrupole mass spectrometry with electrospray ionization (HPLC–MS/MS) and immunoaffinity column chromatography were used for extraction and purification of aflatoxins. PDA media was selected for fungal count. Results: A good quality linear relationship was originated for AFB1, AFB2, AFG1 and AFG2 at 1–10 ppb (r > 0.9995). The analyte precision at three different spiking levels was 88.7–109.1 %, by means of low per cent relative standard deviations in each case. Within 5 to7 min aflatoxins can be separated using an Agilent XDB C18-column. We found that AFB1 and AFB2 were not found in D. denudatum. This was reliable through exceptionally low figures of fungal colonies observed after 6 hr of incubation. The developed analytical method is straightforward, be successfully used to determine the aflatoxins. Conclusion: The developed analytical method is straightforward, simple, accurate, economical and can be successfully used to find out the aflatoxins in remedial plants and consequently to have power over the quality of products. The presence of aflatoxin in the plant extracts was interrelated to the least fungal load in the remedial plants examined.

Keywords: aflatoxins, delphinium denudatum, liquid chromatography, mass spectrometry

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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: Evgeny E. Tereshatov

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Astatine-211 is considered one of the most promising radionuclides for Targeted Alpha Therapy. In order to develop reliable procedures to label biomolecules and utilize efficient delivery vehicle principles, one should understand the main chemical characteristics of astatine. The short half-life of 211At (~7.2 h) and absence of any stable isotopes of this element are limiting factors towards studying the behavior of astatine. Our team has developed a procedure for rapid and efficient isolation of astatine from irradiated bismuth material in nitric acid media based on 3-octanone and 1-octanol extraction chromatography resins. This process has been automated and it takes 20 min from the beginning of the target dissolution to the At-211 fraction elution. Our next step is to consider commercially available chromatography resins and their applicability in astatine purification in the same media. Results obtained along with the corresponding sorption mechanisms will be discussed.

Keywords: astatine-211, chromatography, automation, mechanism, radiopharmaceuticals

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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: R. Mickiene, A. Friese, U. Rosler, A. Maruska, O. Ragazinskiene

Abstract:

This research focuses on phytochemistry and antimicrobial activities of compounds isolated and identified from three species of Eryngium. The antimicrobial activity of extracts from Eryngiumplanum L., Eryngium maritimum L., Eryngium campestre L. grown in Lithuania, were tested by the method of series dilutions, against different bacteria species: Escherichia coli, Proteus vulgaris and Staphylococcus aureus with and without antibiotic resistances, originating from livestock. The antimicrobial activity of extracts was described by determination of the minimal inhibitory concentration. Preliminary results show that the minimal inhibitory concentration range between 8.0 % and 17.0 % for the different Eryngium extracts and bacterial species.The total amounts ofphenolic compounds and total amounts of flavonoids were tested in the methanolic extracts of the plants. Identification and evaluation of the phenolic compounds were performed by liquid chromatography. The essential oils were analyzed by gas chromatography mass spectrometry.

Keywords: antimicrobial activities, Eryngium L. species, essential oils, gas chromatography mass spectrometry

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Authors: Asmaa Mandour, Ramzia El-Bagary, Asmaa El-Zaher, Ehab Elkady

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Background: An UHPLC (ultra high performance liquid chromatography) method for the simultaneous determination of norfloxacin (NOR), metronidazole (MET) and tinidazole (TNZ) using monolithic column is presented. Purpose: The method is considered an environmentally friendly method with relatively low organic composition of the mobile phase. Methods: The chromatographic separation was performed using Phenomenex® Onyex Monolithic C18 (50mmx 20mm) column. An elution program of mobile phase consisted of 0.5% aqueous phosphoric acid : methanol (85:15, v/v). Where elution of all drugs was completed within 3.5 min with 1µL injection volume. The UHPLC method was applied for the stability indication of NOR in the presence of its acid degradation product ND. Results: Retention times were 0.69, 1.19 and 3.23 min for MET, TNZ and NOR, respectively. While ND retention time was 1.06 min. Linearity, accuracy, and precision were acceptable over the concentration range of 5-50µg mL-1for all drugs. Conclusions: The method is simple, sensitive and suitable for the routine quality control and dosage form assay of the three drugs and can also be used for the stability indication of NOR in the presence of its acid degradation product.

Keywords: antibacterial, monolithic cilumn, simultaneous determination, UHPLC

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Authors: Esma Kocaoglu, Oktay Talaz, Huseyin Cavdar, Murat Senturk, Deniz Eki̇nci̇

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Glutathione reductase (GR) is a crucial antioxidant enzyme which is responsible for the maintenance of the antioxidant GSH (glutathione) molecule. Antimalarial effects of some chemical molecules are attributed to their inhibition of GR; thus inhibitors of this enzyme are expected to be promising candidates for the treatment of malaria. In this work, GR inhibitory properties of N-Methylpyrrole derivatives are reported. Firstly, GR was purified by means of affinity chromatography using 2’,5’-ADP-Sepharose 4B as ligand. Enzymatic activity was measured by Beutler’s method. Synthesis of the compounds was approved by thin layer chromatography and column chromatography. Different inhibitor concentrations were used and all compounds were tested in triplicate at each concentration used. It was found that all compounds have better inhibitory activity than the strong GR inhibitor N,N-bis(2-chloroethyl)-N-nitrosourea, especially three molecules, 8m, 8n, and 8q, are the best among them with low micromolar I₅₀ values. Findings of our study indicate that these Schiff base derivatives are strong GR inhibitors which can be used as leads for designation of novel antimalaria candidates.

Keywords: glutathione reductase, antimalaria, inhibitor, enzyme

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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: 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: H. Elgubbi, A. Mlitan, A. Alzridy

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Ninhydrin is the most well known spray reagent for identification of amino acids. Spring with Ninhydrin as a non-specific reagent is well-known and widely used for its remarkable high sensitivity. Using Ninhydrin reagent alone to detect amino acid on thin layer chromatography (TLA) paper is not advisable due to its lower sensitivity. A new spray reagent, Stannus chloride solution (Sn CL2) has been used to detect amino acids on filtter paper (witman 14) and TLC paper, silica Gel, 60 F254 TLC Aluminium Sheet 20x20cm Merck- Germany. Also, modified TLC pre-staining method was used, which only consisted of 3 steps: spotting, separating and color. The improved method was rapid and inexpensive and the results obtained were clear and reliable. In addition, it is suitable for screening different amino acid.

Keywords: amino acid, ninhydrin, modified ninhydrin reagent, stannus chloride reagent, thin-layer chromatography (TLC), TLC pre-staining

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Authors: Methaq Algabr, Nabil Al-Hajj, Ameerh Jaber, Amtellah Alshotobi, Shaima'a Al-suryhi, Gadah Whaban, Nawal Alshehari

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Steam distillation of the essential oil of P. jaubertii was performed using a Clevenger apparatus. Essential oils were analyzed by gas chromatography-flame ionization detector (GC-FID) and gas chromatography coupled to chromatography–mass spectrometry (GC-MS). The major chemical components identified in P. jaubertii essential oil include carvotanacetone (63.975%), 1-methyl-1,2-propanedione (5.887%), 2,5-dimethoxy-para-cymene (3.303%) and ar-curcumene (3.276%). The antimicrobial activity of the essential oil of P. jaubertii was evaluated against all tested microorganisms. P. jaubertii essential oil inhibited all tested microorganisms except Escherichia coli with a minimum inhibitory concentration (MIC) of 5.0 μg/mL against Staphylococcus aureus.

Keywords: Pulicaria jaubertii, essential oil, antimicrobial, Carvotancetone

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Authors: Steffen Happel

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Non-standard isotopes such as Sc-44/47, Zr-89, and Sn-117mare finding interest is increasing in radiopharmaceutical applications. Methods for the separation of these elements from typical target materials were developed. The methods used in this paper are based on the use of extraction chromatographic resins such as UTEVA, TBP, and DGA resin. Information on the selectivity of the resins (Dw values of selected elements in HCl and HNO3 of varying concentration) will be presented as well as results of the method development such as elution studies, chemical recoveries, and decontamination factors. Developed methods are based on the use of vacuum supported separation allowing for fast and selective separation.

Keywords: elution, extraction chromatography, radiopharmacy, decontamination factors

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Authors: George Madalin Danila, Mihaiella Cretu, Cristian Puscasu

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Glycol-based anti-freeze liquids, commonly composed of ethylene glycol or propylene glycol, have important uses in automotive cooling, but they should be handled with care due to their toxicity; ethylene glycol is highly toxic to humans and animals. A fast, accurate, precise, and robust method was developed for the simultaneous quantification of 7 most important glycols and their isomers. Glycols were analyzed from diluted sample solution of coolants using gas-chromatography coupled with mass spectrometry in single ion monitoring mode. Results: The method was developed and validated for 7 individual glycols (ethylene glycol, diethylene glycol, triethylene glycol, tetraethylene glycol, propylene glycol, dipropylene glycol and tripropylene glycol). Limits of detection (1-2 μg/mL) and limit of quantification (10 μg/mL) obtained were appropriate. The present method was applied for the determination of glycols in 10 different anti-freeze liquids commercially available on the Romanian market, proving to be reliable. A method that requires only a two-step dilution of anti-freeze samples combined with direct liquid injection GC-MS was validated for the simultaneous quantification of 7 glycols (and their isomers) in 10 different types of anti-freeze liquids. The results obtained in the validation procedure proved that the GC-MS method is sensitive and precise for the quantification of glycols.

Keywords: glycols, anti-freeze, gas-chromatography, mass spectrometry, validation, recycle

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Authors: Reza Pashaei, Reda Dzingelevičienė

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An efficient, reliable, and sensitive multiclass analytical method has been expanded to simultaneously determine 15 human pharmaceutical residues in fish and shrimp tissue samples by ultra-high-performance liquid chromatography-tandem mass spectrometry. The investigated compounds comprise ten classes, namely analgesic, antibacterial, anticonvulsant, cardiovascular, fluoroquinolones, macrolides, nonsteroidal anti-inflammatory, penicillins, stimulant, and sulfonamide. A simple liquid extraction procedure based on 0.1% formic acid in methanol was developed. Chromatographic conditions were optimized, and mobile phase namely 0.1 % ammonium acetate (A), and acetonitrile (B): 0 – 2 min, 15% B; 2 – 5 min, linear to 95% B; 5 – 10 min, 95% B; and 10 – 12 min was obtained. Limits of detection and quantification ranged from 0.017 to 1.371 μg/kg and 0.051 to 4.113 μg/kg, respectively. Finally, amoxicillin, azithromycin, caffeine, carbamazepine, ciprofloxacin, clarithromycin, diclofenac, erythromycin, furosemide, ibuprofen, ketoprofen, naproxen, sulfamethoxazole, tetracycline, and triclosan were quantifiable in fish and shrimp samples.

Keywords: fish, liquid chromatography, mass spectrometry, pharmaceuticals, shrimp, solid-phase extraction

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Authors: M. Yakoubi, N. Belboukhari, A. Cheriti, K. Sekoum

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Launaea nudicaulis (L.) Hook.f. is a desert, spontaneous plant and endemic to northem Sahara, which belongs to the Asteraceae family. This species exists in the region of Bechar (Local name; El-Rghamma). In our knowledge, no work has been founded, except studies showing the antimicrobial and antifungal activity of methalonic extract of this plant. The present paper describes the chemical composition of the essential oil from Launaea nudicaulis and qualification of isolation and identification of some pure products by column chromatography. The essential oil from the aerial parts of Launaea nudicaulis (Asteraceae) was obtained by hydroditillation in 0.4% yield, led to isolation of four several new products. The isolation is made by column chromatography and followed by GC-IK and GC-MS analysis.

Keywords: Launaea nudicaulis, asteraceae, essential oil, column chromatography, GC-FID, GC-MS

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Authors: A. D. Susanti, W. B. Sediawan, S. K. Wirawan, Budhijanto, Ritmaleni

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Rice bran oil contains significant amounts of oryzanol, a natural antioxidant that considered has higher antioxidant activity than vitamin E (tocopherol). Oryzanol reviewed has several health properties and interested in pharmacy, nutrition, and cosmetics. For practical usage, isolation and purification would be necessary due to the low concentration of oryzanol in crude rice bran oil (0.9-2.9%). Batch chromatography has proved as a promising process for the oryzanol recovery, but productivity was still low and scale-up processes of industrial interest have not yet been described. In order to improve productivity of batch chromatography, a continuous chromatography design namely Simulated Moving Bed (SMB) concept have been proposed. The SMB concept has interested for continuous commercial scale separation of binary system (oryzanol and rice bran oil), and rice bran oil still obtained as side product. Design of SMB chromatography for oryzanol separation requires quantification of its equilibrium. In this study, equilibrium of oryzanol separation conducted in batch adsorption using silica as the adsorbent and n-hexane/acetone (9:1) as the eluent. Three isotherm models, namely the Henry, Langmuir, and Freundlich equations, have been applied and modified for the experimental data to establish appropriate correlation for each sample. It turned out that the model quantitatively describe the equilibrium experimental data and will directed for design of SMB chromatography.

Keywords: adsorption, equilibrium, oryzanol, rice bran oil, simulated moving bed

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Authors: Preeti Panthari, Harsha Kharkwal

Abstract:

Myrica nagi belongs to Myricaceae family. It is known for its therapeutic use since ancient times. The leaves were extracted with methanol and further fractioned with different solvents with increasing polarity. The n-butanol fraction of methanol extract was passed through celite, on separation through silica gel column chromatography yielded ten fractions. For the first time we report isolation of Caffeic acid from n-butanol fraction of Myrica nagi leaves in Chloroform: methanol (70:30) fraction. The mobile phase used for analysis in HPLC was Methanol: water (60:40) at the flow rate of 1 ml/min at wavelength of 280 nm. The retention time was 2.66 mins.

Keywords: Myrica nagi, column chromatography, retention time, caffeic acid

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Authors: Robert van Ling, Alexander Schwahn, Shanhua Lin, Ken Cook, Frank Steiner, Rowan Moore, Mauro de Pra

Abstract:

Purpose: Demonstration of fast high resolution charge variant analysis for monoclonal antibody (mAb) therapeutics within 5 minutes. Methods: Three commercially available mAbs were used for all experiments. The charge variants of therapeutic mAbs (Bevacizumab, Cetuximab, Infliximab, and Trastuzumab) are analyzed on a strong cation exchange column with a linear pH gradient separation method. The linear gradient from pH 5.6 to pH 10.2 is generated over time by running a linear pump gradient from 100% Thermo Scientific™ CX-1 pH Gradient Buffer A (pH 5.6) to 100% CX-1 pH Gradient Buffer B (pH 10.2), using the Thermo Scientific™ Vanquish™ UHPLC system. Results: The pH gradient method is generally applicable to monoclonal antibody charge variant analysis. In conjunction with state-of-the-art column and UHPLC technology, ultra fast high-resolution separations are consistently achieved in under 5 minutes for all mAbs analyzed. Conclusion: The linear pH gradient method is a platform method for mAb charge variant analysis. The linear pH gradient method can be easily optimized to improve separations and shorten cycle times. Ultra-fast charge variant separation is facilitated with UHPLC that complements, and in some instances outperforms CE approaches in terms of both resolution and throughput.

Keywords: charge variants, ion exchange chromatography, monoclonal antibody, UHPLC

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