Journal of Chromatography & Separation Techniques最新文献

{"title":"A Simple and Sensitive High Performance Liquid Chromatographic Method for Estimation of Transitmycin in Plasma","authors":"H. Ak, B Jagdeesh, Sudha","doi":"10.35248/2157-7064.20.11.425","DOIUrl":"https://doi.org/10.35248/2157-7064.20.11.425","url":null,"abstract":"A high performance liquid chromatographic method for estimation of Transitmycin (Tr) in human plasma was developed. The analyte was extracted using solid phase cartridges and the analysis of the eluent was carried out using Atlantis T3 column (150 cm × 4.6 mm ID) and photo diode array detector set at wavelength of 214 nm.  The assay was specific for Tr and linear from 0.5 µg/mL to 20.0 µg/mL. The relative standard deviations for intra- and inter-day assays were less than 10%. The method yielded a recovery for Tr that ranged from 94% to 107% and could be used in toxicology and pharmacokinetic studies.","PeriodicalId":15534,"journal":{"name":"Journal of Chromatography & Separation Techniques","volume":"25 1","pages":"1-4"},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"87357076","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Application of High-Performance Thin Layer Chromatography in the Quantitative Estimation of Serum Clobazam Levels","authors":"R. Kulkarni-Munshi, J. Vishwakarma","doi":"10.35248/2157-7064.20.11.433","DOIUrl":"https://doi.org/10.35248/2157-7064.20.11.433","url":null,"abstract":"This study was aimed to develop and validate a High-Performance Thin Layer Chromatography (HPTLC) method for the quantitative determination of serum clobazam levels. This simple and sensitive method will help in therapeutic drug monitoring that aids in the clinical management of patient therapy. Chromatographic separation was carried out on a silica gel 60F254 HPTLC plate using a mixture of Toluene:Methanol:Glacial acetic acid (15:1:0.16, v/v/v) as the mobile phase. Densitometric detection was carried out at 231 nanometers. The method was validated for specificity, precision, accuracy, robustness, linearity, limit of detection, and limit of quantification. Linear calibration curves in the range of 5-80 microgram per band gave a correlation coefficient of 0.99077. The intra-day (n=6) and inter-day (n=18) precision, expressed as the relative standard deviation were in the range of 0.36 to 4.44% and from 0.76 to 2.13%. Clobazam gave a well separated peak at Retardation factor (Rf) 0.30. Caffeine was used as an internal standard, which gave a well separated peak at Retardation factor (Rf) 0.20 without interfering with clobazam. The method was found to be specific with no matrix interference. Thus, the method developed for the estimation of serum clobazam level is simple, cost-effective and reliable for therapeutic drug monitoring.","PeriodicalId":15534,"journal":{"name":"Journal of Chromatography & Separation Techniques","volume":"15 1","pages":"1-4"},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82604648","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"High-Performance Liquid Chromatography with Diode Array Detection for the Simultaneous Quantification of Piperaquine and Mefloquine in Human Plasma in Vietnamese Uncomplicated Malaria Patients","authors":"Pham Van Toi, Truong Le Phuc Nhi, N. H. Chau, Nguyen Thanh Tong, G. Thwaites, T. Hien","doi":"10.35248/2157-7064.20.11.430","DOIUrl":"https://doi.org/10.35248/2157-7064.20.11.430","url":null,"abstract":"A bioanalytical method using high-performance liquid chromatography with diode array detection was developed and validated for quantification of piperaquine and mefloquine in human plasma. After extraction from 200 μL of plasma by using solid phase extraction on MCX-96 well plate; piperaquine, mefloquine and quinine (internal standard) were separated using a mobile phase consisting of trichloroacetic acid 1 mM and trimethylamine 0.025%, pH 3.4-Acetonitrile applying gradient elution on a Poroshell 120, C8 end capped 100 × 4.6 mm, 2.7 μm column at a flow rate of 1.0 mL/min at 35°C. The peaks were monitored with a diode array detection set at a wavelength of 343 nm for piperaquine, quinine and 283 nm for mefloquine. The limit of quantification was 10 ng/mL, 50 ng/ mL for piperaquine and mefloquine, respectively. The method was linear over the range of 10 to 2,000 ng/ml for piperaquine and 50 to 10,000 ng/ml for mefloquine in plasma. The intra, inter assay precision were less than 8% overall quality control ranges for these analytes. The accuracies varied between 99.85% and 104.6% at all quality control levels for piperaquine and mefloquine. The validated method was applied to measure the concentrations of piperaquine, mefloquine in samples collected from 12 uncomplicated malaria patients in Binh Phuoc province, Vietnam.","PeriodicalId":15534,"journal":{"name":"Journal of Chromatography & Separation Techniques","volume":"1 1","pages":"1-9"},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"89365627","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Recent Developments in Gas Chromatography-Mass Spectrometry","authors":"T. Fujino","doi":"10.35248/2157-7064.20.S1.426","DOIUrl":"https://doi.org/10.35248/2157-7064.20.S1.426","url":null,"abstract":"","PeriodicalId":15534,"journal":{"name":"Journal of Chromatography & Separation Techniques","volume":"71 1","pages":"1-2"},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"80703192","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Gas Chromatography-Mass Spectrometry (GC-MS) Profiling of Hops and Some Nigerian Potential Hop Substitutes: Comparative Studies in Beer Brewing","authors":"V. Okafor, U. W. Okafor, R. I. Anyalebechi","doi":"10.35248/2157-7064.20.11.429","DOIUrl":"https://doi.org/10.35248/2157-7064.20.11.429","url":null,"abstract":"Isomerized hop extract and methanolic extracts of Azadirachta indica, Garcinia kola, Gongronema latifolium and Vernonia amygdalina were profiled by the application of Gas Chromatography-Mass Spectrometry (GC-MS). The isomerized hop extract and ethanolic extracts of the plant species were used to brew beers. The aim was to study the GC-MS profiles of all the extracts comparatively and to investigate some physicochemical properties of beers brewed with hop extracts and in comparison, with beers brewed with extracts from the four Nigerian plants. The profiling of the metabolites in hop extracts and those of the Nigerian plants was carried out using Gas Chromatography - Mass Spectrometer. The physicochemical properties of the finished beer products were also carried out using standard methods. Beers brewed with extracts from the Nigerian plants were statistically ranked by the application of Analysis of Variance (ANOVA) to ascertain their potentiality. The GCMS results showed that these plants contained metabolites comparable to those of hops, although some metabolites [dehydro-cohumulunic acid; 4,4-dimethyl- 2-buten-4-olide; 1,2-dimethyl-cyclopropane carboxylic acid; lupulone; 2,5-dimethyl-2-hexanol; 4,4,5,5-tetramethylbicyclo hexyl-6-ene-2,3-dione; octadecanoic acid, oxiranyl methyl ester and 1,2-benzenedicarboxylic, bis(-2-ethyl hexyl) ester] present in hops were absent in the Nigerian plants. Isomerized hop, hop leaf, G. kola and V. amygdalina extracts contained 14, 11, 12 and 9 metabolites respectively while those of A. indca and G. latifolium contained 10 metabolites each. The physicochemical properties of the brewed beers revealed that the alcohol content in all the beer samples ranged from 3.43-3.75%, total acidity (0.132-0.324%), pH (5.47-5.68), turbidity (5-125NTU), total solids (3.66- 8.16%) and bitterness level (25.38-39.62IBU). The concentration of arsenic in the beer samples ranged from 1.44- 1.77ppm, cadmium (0.00-0.97ppm) and copper (0.10-2.70ppm). Test of significant (p-value) in all the tested plants was greater than 0.05 at 95% confidence interval. Consequently, the extracts from tested Nigerian plants could be used as suitable substitutes for hops in beer brewing without alteration of physicochemical properties of beer, G. kola having the greatest potential as substitute for hops.","PeriodicalId":15534,"journal":{"name":"Journal of Chromatography & Separation Techniques","volume":"1 1","pages":"1-9"},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"84009282","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Distribution and Source of Polycyclic Aromatic Hydrocarbons in Water and Sediments from Egbe Dam in Southwestern Nigeria","authors":"O. Ibigbami, S. Asaolu, Popoola Ok, S. Adefemi, Abodunde Ts, K. Idowu, Olatoye Ro","doi":"10.35248/2157-7064.20.11.424","DOIUrl":"https://doi.org/10.35248/2157-7064.20.11.424","url":null,"abstract":"Egbe dam is capable of supplying potable water to the whole Ekiti State. The need for water quality is not just to protect the public health but also to support the economy and maintain a rich ecosystem. The aim of this study was to assess the level of polycyclic aromatic hydrocarbons (PAHs) in surface water and sediments of Egbe dam and also to investigate their sources using profiles and ratios. A gas chromatography (GC) coupled with flame ionization detector (FID) was used for PAHs identification and quantification after careful extraction and clean-up. The results showed the presence of the studied PAHs except naphthalene with mean concentration range of 0.009 mg/L (fluorene)-1.08 mg/L (benzo(a)pyrene) and 0.071 mg/Kg (phenanthrene)-1.37 mg/Kg (benzo(a)anthracene) in water and sediments respectively. The coefficient of variation revealed high spatial variation in the PAHs distribution level with the predominance of high molecular PAHs. The results reflected high percentage (91.6%) levels of HMW-PAHs as compared to LMW-PAHs. Some samples exceeded the compared PAHs international standard guidelines for groundwater and drinking water. Sources identification showed that the PAHs are pyrogenic. The detectable amounts of PAHs in the dam make it inevitable to conduct regular monitoring so as to ensure that the levels remain below prescribed limits by national and international standards.","PeriodicalId":15534,"journal":{"name":"Journal of Chromatography & Separation Techniques","volume":"440 1","pages":"1-7"},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"82911427","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Determination of Neonicotinoid (Nitenpyram, Imidacloprid and Acetamiprid) Pesticides Residues in Five Dried Vegetables by High Performance Liquid Chromatography","authors":"M. Sajid, M. Razzaq, Z. Ali, Dilshad Hussain, A. Hussain, A. Yar, M. Hayat","doi":"10.35248/2157-7064.20.11.431","DOIUrl":"https://doi.org/10.35248/2157-7064.20.11.431","url":null,"abstract":"A method using dispersive solid-phase extraction (d-SPE) cleanup followed by QuEChERS with High Performance Liquid Chromatography (HPLC) has been established for determination of Neonicotinoid pesticide residues in various vegetables including brinjal, salad leaves, coriander, cabbage and lady finger. Based on an assessment of the HPLC characteristics, validation experiments are conducted for three Neonicotinoid pesticides i.e. Nitenpyram, Imidacloprid and Acetamiprid. In acidified acetonitrile analytical extraction is done with NaCl and MgSO4 followed by activated neutral carbon. The method show good linearity (R2 ≥ 0.999) and relative standard deviation (RSD ≤ 3.36%). Average recoveries of three insecticides are in the range of 55% to 82% at spiking levels of 275.68 to 409.3 mg.Kg-1. LOD and LOQ of three Neonicotinoid pesticides are in the range of 2.658 - 3.761 mg.Kg-1 and 8.056 - 11.4 mg.Kg-1. This QuEChERS determination method by HPLC is precise, simple, sensitive, accurate, easy to perform, and diversified at slightly higher concentrations. Moreover, it is very efficient and effective method and it can be utilized for regular monitoring of pesticide residues in drinking, canal and river water to save the life of organisms and to keep the aquatic environment clean.","PeriodicalId":15534,"journal":{"name":"Journal of Chromatography & Separation Techniques","volume":"20 1","pages":"1-7"},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"74973893","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Simultaneous Quantitative Determination of Synthetic Cathinone Enantiomers in Urine by GC-NCI-MS/MS using Menthylchloroformate as Chiral Derivatization Reagent","authors":"Mohammed A Meetani, Alzaabi Ja, S. Hisaindee, Altabaji Mk, R. Alremeithi","doi":"10.35248/2157-7064.20.11.436","DOIUrl":"https://doi.org/10.35248/2157-7064.20.11.436","url":null,"abstract":"Development and validation of a new analytical method for enantioseparation and quantitation of synthetic cathinones is reported using a chiral derivatization agent (CDA) and GC-MS triple quadrupole mass spectrometry with negative chemical ionization (NCI) mode. Indirect separation of ten synthetic cathinone compounds has been achieved using a commercially available optically pure CDA called (1R)-(-)-menthylchloroformate (MCF). MCF was capable of converting synthetic cathinone enantiomers into diastereoisomers, which were later separated with good resolution on an ultra-inert 60 m achiral stationary phase column. An internal standard (IS), 3-methylmethcathinone (3-MMC) was used for quantitation of synthetic cathinone diastereoisomers. Method validation in terms of calibration curve linearity, sensitivity in terms of limits of detections (LODs), limits of quantitation (LOQs), interday and intra-day reproducibility, and recoveries has been obtained for the ten synthetic cathinone compounds that were analyzed simultaneously as a mixture after being spiked in urine. It was found that LOD’s and LOQ’s for the ten synthetic cathinones mixture in urine were in the ranges of 0.004-3.678 ppm and 0.012-11.14 ppm respectively. The results of four synthetic cathinones (Buphedrone, 3-MethylBP,3,4-DMEC, and Butylone) derivatized with MCF were compared with the same compounds derivatized with N-trifluoroacetyl-L-prolyl chloride (L-TPC). It was found that the later was more sensitive in terms of LOD and LOQ than the former method.","PeriodicalId":15534,"journal":{"name":"Journal of Chromatography & Separation Techniques","volume":"77 1","pages":"1-8"},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81138326","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"A Rapid Technique for Plant Peptides Isolation Based on their Polarity by Using BIOTAGE Isolera One Flash Chromatography","authors":"E. M. Bedikou, R. Logesh, S. Niamké, Palaniswamy Dhanabal","doi":"10.35248/2157-7064.20.11.427","DOIUrl":"https://doi.org/10.35248/2157-7064.20.11.427","url":null,"abstract":"Several years of experience performing columns chromatography have been condensed into simple guidelines useful for translating thin layer chromatography (TLC) results into either isocratic- or gradient-flash chromatography. The present study describes the use of such protocol with a silica Biotage SNAP KP-Sil 10 g cartridge (21 mm A— 55 mm, 50 I¼m particle size), to purify, in a single step, four (4) peptides from crude proteins extract of germinated Amaranthus hybridus seeds. The best solvent system used was a combination of n-hexane (non-polar solvent B from 5% to 0% final concentration) and a mixture of polar solvents (solvent A) composed of acetonitrile, n-butanol, glacial acetic acid and water in 0.9:2:1:1 ratio, respectively. The elution was done in normal-phase with a linear gradient. All the flash chromatography procedure took at most twenty-five minutes (25 min), and less than a liter (750 mL) of total solvents was used. The purified peptides named AhPA, AhPB, AhPC and AhPE showed apparent homogeneity on TLC plates, and purification yields of about 11.15%, 10.38%, 14.50% and 17.25%, respectively. This innovative technique provides an efficient alternative to researchers’ in peptides purification and participates in reducing the waste of solvents, gels, time and thus, money.","PeriodicalId":15534,"journal":{"name":"Journal of Chromatography & Separation Techniques","volume":"119 1","pages":"1-5"},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"77455550","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}

{"title":"Adsorption of Phenolic Compounds from an Aqueous By-product of Sunflower Protein Extraction/Purification by Macroporous Resins","authors":"Tuong Vy. Le Thi, Arnaud Aymes, X. Framboisier, I. Ioannou, R. Kapel","doi":"10.35248/2157-7064.20.11.435","DOIUrl":"https://doi.org/10.35248/2157-7064.20.11.435","url":null,"abstract":"In this study, adsorption of phenolic compounds from an aqueous by-product of sunflower protein isolate production was investigated. Phenolic compounds in this by-product (ultrafiltration permeate of protein purification step) were almost exclusively CGA (mainly 5-CQA isomer). Five different macroporous resins including XAD4, XAD7, XAD16, XAD1180, and HP20 were screened for CGA capture. XAD16 had the best massic adsorption capacities (15.32 ± 0.04 mg/g), while XAD7 had a better surface adsorption capacity (0.027 ± 0.00146 mg/m²). CGA adsorption on both resins followed the pseudo-second-order kinetic model with a similar intra diffusional pattern. Adsorption isotherms of the two resins better fitted the Langmuir model with Qmax for XAD7 and XAD16 of 0.054 and 0.040 (mg/m²), respectively. The adsorption process of phenolic compounds revealed to be exothermic, physical adsorption, and spontaneous. Better adsorption results were observed at 25°C. Maximal CGA desorption ratio was observed from 70% (v/v) ethanol. The high values were reached with both the resins (88.09 ± 0.13 and 86.16 ± 0.32% for XAD7 and XAD16, respectively). The CGA purity in the desorption phase was surprisingly high (77.56 ± 0.99% and 74.59 ± 0.12% for XAD7 and XAD16, respectively).","PeriodicalId":15534,"journal":{"name":"Journal of Chromatography & Separation Techniques","volume":"4 1","pages":"435"},"PeriodicalIF":0.0,"publicationDate":"2020-01-01","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":null,"resultStr":null,"platform":"Semanticscholar","paperid":"81662293","PeriodicalName":null,"FirstCategoryId":null,"ListUrlMain":null,"RegionNum":0,"RegionCategory":"","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":"","EPubDate":null,"PubModel":null,"JCR":null,"JCRName":null,"Score":null,"Total":0}