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Journal of Chromatographic Science

Wu Chen, Anne Mack, Bo Sachok, Kunqiang Jiang, Xiaoli Wang
In this study, we studied the chromatographic performance of this newly developed wide pore superficially porous particles (SPPs) with 3.5 μm particle size and 450 Å pore size, for the separation of proteins and Immunoglobulin G antibodies. We studied the selectivity of different phases (C4, SB-C18 and Diphenyl), the effect of temperature, column carryover and column chemical lifetime. We also compared our SPPs with other wide pore SPPs in similar particle sizes and sub 2 µ wide pore totally porous particles by van Deemter studies and gradient separations of proteins and immunoglobulin G antibodies...
March 7, 2018: Journal of Chromatographic Science
Min Yang, Zhonghua Dong, Xiaoyan Jiang, Zhongxi Zhao, Jianqiang Zhang, Xinke Cao, Daizhou Zhang
In this work, a rapid, simple, sensitive and specific LC-MS/MS method was developed and validated for the quantification of S-Allylmercaptocysteine (SAMC) in plasma. After a simple sample procedure by one step protein precipitation with acetontrile, the samples were separated on Gemini-NX C18 column (2.1 mm i.d. 150 mm, 3 μm, Phenomenex). The mobile phase was composed of water-acetonitrile (20:80, v/v) at an isocratic flow rate of 0.3 mL/min. The developed method was validated based on the International Conference on Harmonization (ICH) guidelines...
March 7, 2018: Journal of Chromatographic Science
Reem N El Gammal, Mohammed E A Hammouda, Dalia R El-Wasseef, Saadia M El-Ashry
A simple rapid and accurate micellar high performance liquid chromatographic method was improved and validated for the analysis of mixture containing gatifloxacin sesquihydrate (GTF) and prednisolone acetate (PRED) in their synthetic mixture and their combined preparation. The separation was achieved using a C18 column, micellar mobile phase consisted of 0.2 M sodium dodecyl sulfate, 12.5% n-propanol and 0.3% triethylamine in 0.02 M orthophosphoric acid at pH 7.0 at a flow rate of 1 ml/min with UV detection at 270 nm...
February 21, 2018: Journal of Chromatographic Science
R Siva Kumar, K V Sravan Kumar, L Kondareddy, K R Yogeshwara, Gangrade Manish, Jayachandran Jeenet, Kanyawar Nitesh
A new sensitive and stability indicating reverse phase high-performance liquid chromatography method has been developed for the quantitative determination of potential impurities of Ledipasvir, active pharmaceutical ingredient. Efficient chromatographic separation was achieved on waters × select column contains C18 stationary phase in gradient mode, quantitation at wavelength of 325 nm and mobile phase A is 50 mM ammonium formate pH 3.5 and mobile phase B is acetonitrile with flow rate 1.2 mL. The method was validated according to International Council for Hormonisation guideline, linearity studies has shown correlation coefficient value greater than 0...
February 21, 2018: Journal of Chromatographic Science
Khalid A M Attia, Nasr M El-Abasawi, Ahmed El-Olemy, Ahmed H Abdelazim
Lesinurad is a novel selective uric acid reabsorption inhibitor which has been newly approved for the treatment of the chronic gout. The behavior of lesinurad under various stress conditions (hydrolysis, oxidation, thermal and photolysis) has been investigated as per ICH guidelines. The drug has been found to be labile to acidic hydrolysis, basic hydrolysis and oxidation but stable in neutral, thermal and photolytic conditions. A high performance liquid chromatographic method has been developed for selective determination of the studied drug in the presence of its related degradation products...
February 21, 2018: Journal of Chromatographic Science
Beata Morak-Mlodawska, Krystian Pluta, Malgorzata Jelen
The lipophilicity of new two series of anticancer active 10-substituted 1,6- and 3,6-diazaphenothiazines has been investigated using reversed-phase thin-layer chromatography. Their lipophilicity (RM0 and log PTLC) was determined with mixtures of acetone and Tris buffer as mobile phases. The relative lipophilicity parameter RM0 and specific hydrophobic surface area b were significantly intercorrelated showing congeneric classes of diazaphenothiazines. The parameter RM0 was transformed into parameter log PTLC by use of the calibration curve...
February 7, 2018: Journal of Chromatographic Science
Michael O Gaylor, Hope L Juntunen, Donna Hazelwood, Patrick Videau
Considerable effort has been devoted to analytical determinations of sugar and amino acid constituents of plant nectars, with the primary aim of understanding their ecological roles, yet few studies have reported more exhaustive organic compound inventories of plant nectars or extrafoliar nectars. This work evaluated the efficacy of four solvents (ethyl acetate, dichloromethane, toluene and hexane) to extract the greatest number of organic compound classes and unique compounds from extrafoliar nectar drops produced by Sansevieria spp...
February 7, 2018: Journal of Chromatographic Science
A Hemdan, Omar Abdel-Aziz
Run time is a predominant factor in HPLC for quality control laboratories especially if there is large number of samples have to be analyzed. Working at high flow rates cannot be attained with silica based particle packed column due to elevated backpressure issues. The use of monolithic column as an alternative to traditional C-18 column was tested for fast separation of pharmaceuticals, where the results were very competitive. The performance comparison of both columns was tested for separation of anti-diabetic combination containing Metformin, Pioglitazone and Glimepiride using Gliclazide as an internal standard...
February 7, 2018: Journal of Chromatographic Science
Mariana de Oliveira Almeida, Christian Fernandes, Gerson Antônio Pianetti, Isabela Costa César
Association of amlodipine besylate and olmesartan medoxomil in fixed-dose combination tablets is effective, safe and well tolerated for the treatment of hypertension. The aim of this study was to optimize and validate a novel and fast UHPLC-DAD method for simultaneous quantification of these antihypertensive drugs in tablets, using a transfer procedure from a conventional HPLC-DAD method. The HPLC separation was carried out using a C18 column (150 × 4.6 mm2; 5 μm) and a mobile phase composed of acetonitrile, methanol and 0...
February 2, 2018: Journal of Chromatographic Science
Libin Wang, Jun Zhao, Ruitao Zhang, Le Mi, Xin Shen, Nan Zhou, Tian Feng, Juan Jing, Xueying Liu, Shengyong Zhang
Currently, patients with co-infection with HIV and tuberculosis are treated with more than one drug. PA-824 a new chemical entity and a member of a class of compounds known as nitroimidazo-oxazines, has significant antituberculosis activity and a unique mechanism of action. Darunavir (PrezistaTM) is a new protease inhibitor of HIV-1. A simple, sensitive and rapid LC-MS-MS method has been developed and validated for simultaneous determination of PA-824 and darunavir. Chromatographic separation was achieved on Agilent Eclipse plus C18 column (100 mm × 2...
January 24, 2018: Journal of Chromatographic Science
Mustafa Cittan, Ali Çelik
A simple method was validated for the analysis of 31 phenolic compounds using liquid chromatography-electrospray tandem mass spectrometry. Proposed method was successfully applied to the determination of phenolic compounds in an olive leaf extract and 24 compounds were analyzed quantitatively. Olive biophenols were extracted from olive leaves by using microwave-assisted extraction with acceptable recovery values between 78.1 and 108.7%. Good linearities were obtained with correlation coefficients over 0.9916 from calibration curves of the phenolic compounds...
January 24, 2018: Journal of Chromatographic Science
Vasanti M Suvarna, Preeti C Sangave
Darunavir ethanolate (DRV) is an efficient protease inhibitor (PI) used in the treatment of human immunodeficiency virus (HIV) type-1 patients. An isocratic reversed-phase HPLC method was developed to monitor concentration of darunavir in in vitro intestinal fluid samples in everted sac absorption model in the presence of bioenhancers, viz., piperine, quercetin, naringenin. The method was validated and successfully applied to everted sac and pharmacokinetic studies in rats. The absorption profiles of DRV and apparent permeability coefficients were determined...
January 12, 2018: Journal of Chromatographic Science
Maha M Abdelrahman, Ibrahim A Naguib, Mohamed R El Ghobashy, Nesma A Ali
Two accurate, sensitive and highly selective stability-indicating methods are developed and validated for simultaneous determination of Agomelatine (AGM) and its forced degradation products (Deg I and II). The first method is High-Performance Liquid Chromatography for separation and quantitation of AGM, Deg I and II on a C18 column (250 mm × 4.6 mm, 5 μm p.s) in isocratic mode by using a binary mixture of Potassium dihydrogen phosphate (0.05 M, pH adjusted to 2.9 with orthophosphoric acid): acetonitrile (60:40, v/v) at a flow rate of 2 mL/min...
January 12, 2018: Journal of Chromatographic Science
Francisco Oiram Filho, Daniel Barbosa Alcântra, Tigressa Helena Soares Rodrigues, Lorena Mara Alexandre E Silva, Ebenezer de Oliveira Silva, Guilherme Julião Zocolo, Edy Sousa de Brito
Cashew nut shell liquid (CNSL) contains phenolic lipids with aliphatic chains that are of commercial interest. In this work, a chromatographic method was developed to monitor and quantify anacardic acids (AnAc) in CNSL. Samples containing AnAc were analyzed on a high-performance liquid chromatograph coupled to a diode array detector, equipped with a reversed phase C18 (150 × 4.6 mm × 5 μm) column using acetonitrile and water as the mobile phase both acidified with acetic acid to pH 3.0 in an isocratic mode (80:20:1)...
December 29, 2017: Journal of Chromatographic Science
Qiang Zhou, He Yan, Rui Li, Xingliang Li, Jingyan Wei
1,6-O,O-Diacetylbritannilactone is a natural sesquiterpene lactone isolated from Inula britannica that has displayed cytotoxic effects against several human cancer cell lines. In this study, a selective and sensitive liquid chromatography-tandem mass spectrometry (LC-MS-MS) method was developed for determination of 1,6-O,O-diacetylbritannilactone in rat plasma. Chromatographic separation was achieved on an Agilent C18 column (4.6 mm × 75 mm, 3.5 μm) with methanol and water (80:20, v/v) as the mobile phase...
December 29, 2017: Journal of Chromatographic Science
Rania A Sayed, Manal M El-Masri, Wafaa S Hassan, Magda Y El-Mammli, Abadalla Shalaby
Two novel stability-indicating TLC densitometric and chemometric methods were developed for the determination of mometasone furoate (MF) in the presence of its alkaline degradation product (MF Deg). The developed TLC densitometric method (Method A) is based on the quantitative densitometric separation of MF from its alkaline degradation product on silica gel 60 F254 and measurement of the bands at 250 nm. The separation was carried out using hexane-chloroform-methanol-acetonitrile (6:6:1:0.3, by volume) as a developing system...
December 29, 2017: Journal of Chromatographic Science
Thomas S Thompson, Johan P van den Heever, Stephen F Pernal
Dicyclohexylamine (DCH) is an excipient present in commercial formulations of fumagillin (Fumagilin-B® and Fumidil-B®), an antibiotic which is employed in apiculture for the control of nosema disease. DCH has been demonstrated to be stable in harvested honey; however, its fate in the beehive has not been investigated. In this study, DCH residues were determined in beeswax samples collected from brood chambers and honey supers from various apiaries throughout Alberta. The determination of DCH was performed using a simple extraction procedure followed by low-temperature cleanup and finally analysis with aqueous normal phase liquid chromatography-electrospray ionization tandem mass spectrometry...
December 29, 2017: Journal of Chromatographic Science
Murali Krishna V V N Mantripragada, Sumathi V Rao, Venugopal V S Nutulapati, Bhaskara P V Mantena
A simple, rapid, selective and stability indicating reversed phase-ultra performance liquid chromatography method was developed and validated for the simultaneous quantification of process related and degradation impurities present in Atazanavir and Ritonavir tablets. The two proposed drug components and their respective impurities were separated using Acquity BEH C18 (100 mm × 2.1 mm), 1.7 μ column at a flow rate of 0.4 mL/min. Buffer used as Mobile phase-A which consists of 0.01 M monobasic potassium hydrogen phosphate adjusted the pH to 3...
December 29, 2017: Journal of Chromatographic Science
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December 26, 2017: Journal of Chromatographic Science
Heshuang Dai, Zhiqiong Chen, Bing Shang, Qinhua Chen
A gas chromatographic-mass spectrometric (GC-MS) method was developed for the determination of four anthraquinones found in rhubarb. Chrysophanol, physcion, aloe-emodin and emodin were confirmed by GC-MS and the possible main cleavage pathways of fragment ions are discussed in this study. Rhubarb is a traditional Chinese medicinal herb which required an effective evaluation method to quantitate the four major active anthraquinone compounds described. The determinations of analytes were accomplished by GC-MS using osthole as an internal standard...
March 1, 2018: Journal of Chromatographic Science
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