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1
Continuous separation of protein loaded nanoparticles by simulated moving bed chromatography.
e-Kitap

e-Kitap Open Access
Kaynak :
Internet Archive Books
Yayıncı :
Journal of Chromatography. a
Yazar(lar) :
Alois Jungbauer , Martin Wellhoefer , Peter Satzer
Yıl :
2014
Journal of Chromatography. a
Yayıncı Web Sitesi Tam Metin
Kaydet
This article is from Journal of Chromatography. a, volume 1349. Abstract •Size exclusion chromatography is a general method for nanoparticles separation.•The method is suited for purifying large quantities of protein covered nanoparticles.•Nanoparticles and proteins can be continuously separated by simulated moving bed chromatography.•Particle and protein fractions reached a purity of > 90%.•Reuse of buffer and unbound protein was possible using tangential flow filtration.
DOI : doi:10.1016/j.chroma.2014.04.093
Cilt :1349
ISSN :0021-9673
2
Optimised concentration and purification of retroviruses using membrane chromatography.
e-Kitap

e-Kitap Open Access
Kaynak :
Internet Archive Books
Yayıncı :
Journal of Chromatography. a
Yazar(lar) :
NKH Slater , PR Levison , F Farzaneh , D Darling , DJ McNally
Yıl :
2014
Journal of Chromatography. a
Yayıncı Web Sitesi Tam Metin
Kaydet
This article is from Journal of Chromatography. a, volume 1340. Abstract •An in investigation in to the use of membrane chromatography for the purification of a γ-retrovirus was undertaken.•The first report of a capacity for γ-retrovirus binding to a membrane chromatography device is presented.•A process that produces a large increase in concentration and purity of the studied γ-retrovirus was identified.•Proteomic techniques were used to identify the protein impurities removed and co-purified with the virus containing eluate.
DOI : doi:10.1016/j.chroma.2014.03.023
Cilt :1340
ISSN :0021-9673
Sınıflandırma :
3
Calixarene-immobilized monolithic cryogels for preparative protein chromatography
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Dergi Makalesi
Kaynak 1:
DSpace Makaleler
Kaynak 2:
DSpace Makaleler
Kaynak 3:
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
Journal of Chromatography A
Yazar(lar) :
İdris Güven , Orhan Gezici , Mevlüt Bayrakcı , Massimo Morbidelli
Konu :
Calixarene, Cation-Exchange, Cryogel, Monolithic Column, Separation, Stationary Phase
Yıl :
2018
Journal of Chromatography A
Kaydet
New cation exchanger monolithic stationary phases were prepared by immobilization of three different calixarene derivatives (i.e. tetracarboxylate calix[4]arene, CLX-COO, tetrasulfonate calix[4]arene, CLX-SO3, and tetraphosphonate calix[4]arene, CLX-PO4) onto a monolithic cryogel support (i.e. poly(2-hydroksyethylmethacrilate-co-glycidyl methacrylate, P) and investigated with respect to preparative protein chromatography. The obtained monoliths were characterized through various techniques such as FTIR spectroscopy, isoelectric point measurements, titrimetric analyses, and mercury intrusion porosimetry. Protein retention was investigated using some model proteins (i.e. lysozyme, cytochrome c, and alpha-chymotrypsinogen A, human serum albumin, and myoglobin), and the role of modifier (i.e. NaCI) concentration and pH was thoroughly analyzed under isocratic and gradient elution conditions. Overloading experiments were also conducted to study dynamic adsorption capacity and the obtained values were found to be ranging between 3 and 8 mg/mL depending on the type of calixarene molecule. Hence, higher or comparable protein adsorption capacities were seen to be applicable on calixarene-immobilized cryogels when compared to any other functionalized cryogels in the literature. Combined with the favorable properties of these monoliths, with respect to mass transport of large molecules, these results qualify calixarene functionalized monolithic cryogels as promising stationary phases for protein preparative purification. (C) 2018 Elsevier B.V. All rights reserved.
Anahtar Kelimeler : Calixarene, Cation-Exchange, Cryogel, Monolithic Column, Separation, Stationary Phase, article
Cilt: 1558
ISSN: 0021-9673
Sınıflandırma :
Kimya %100
Kromatografi %100
4
Strong cation-exchange chromatography of proteins on a sulfoalkylated monolithic cryogel
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Dergi Makalesi
Kaynak 1:
DSpace Makaleler
Kaynak 2:
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
Isik Percin , Rushd Khalaf , Bastian Brand , Massimo Morbidelli , Orhan Gezici
Konu :
Gradient elution, HPLC, Ion-exchange, Protein, Separation, Yamamoto Model
Yıl :
2015
JOURNAL OF CHROMATOGRAPHY A
Kaydet
A new strong cation exchanger (SCX) monolithic column was synthesized by at-line surface modification of a cryogel prepared by copolymerization of 2-hydroxyethylmethacrylate (HEMA) and glycidyl-methacrylate (GMA). Sodium salt of 3-Mercaptopropane sulfonic acid (3-MPS) was used as the ligand to transform the surface of the monolith into a strong cation exchanger. The obtained material was characterized in terms of elemental analysis, infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Brunauer-Emmett-Teller (BET) N-2 adsorption, and used as a stationary phase for strong-cation exchange chromatography of some proteins, such as a-chymotrypsinogen, cytochrome c and lysozyme. Water permeability of the column was calculated according to Darcys law (2.66 x 10(-13) m(2)). The performance of the monolithic cryogel column was evaluated on the basis of Height Equivalent to a Theoretical Plate (HETP). Retention behavior of the studied proteins was modeled on the basis of Yamamoto model to understand the role of the ion-exchange mechanism in retention behaviors. The considered proteins were successfully separated, and the obtained chromatogram was compared with that obtained with a non-functionalized cryogel column. (c) 2015 Elsevier B.V. All rights reserved.
Anahtar Kelimeler : Gradient elution, HPLC, Ion-exchange, Protein, Separation, Yamamoto Model, article
Cilt: 1386
ISSN: 0021-9673
Sınıflandırma :
Kimya %100
Kromatografi %94
5
Estimation of measurement uncertainty of polychlorinated biphenyls, polycyclic aromatic hydrocarbons and organochlorine pesticides in the atmosphere using gas chromatography-mass spectrometry and gas chromatography-electron capture detector
Dergi Makalesi

Dergi Makalesi
Kaynak 1:
DSpace Makaleler
Kaynak 2:
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
Journal Of Chromatography A
Yazar(lar) :
Guler Aslan-Sungur , Eftade O. Gaga , Serpil Yenisoy-Karakas
Konu :
Gas chromatography, Polychlorinated biphenyls, Organochlorine pesticides, Polycyclic aromatic hydrocarbons, Air samples, Uncertainty
Yıl :
2014
Journal Of Chromatography A
Kaydet
Estimation of uncertainty of measurement is a crucial issue to achieve accurate measurement results. When the target has adverse environmental and health effects, accuracy of the results become more important. POPs are the pollutants that have toxic effects and unfortunately, there is a lack of information about uncertainty of the method for determining POPs in air samples. In this work, uncertainty calculations were carried out for PCBs, OCPs, and PAHs in air samples analyzed by using GC-MS and GC-ECD. The main dominant sources for combined uncertainty were calibration curve, recovery and repeatability. The relative uncertainties were found to be in the range of 23-52% for PCBs, 24-59% for OCPs and 23-90% for PAHs. (C) 2013 Elsevier B.V. All rights reserved.
Anahtar Kelimeler : Gas chromatography, Polychlorinated biphenyls, Organochlorine pesticides, Polycyclic aromatic hydrocarbons, Air samples, Uncertainty, article
Cilt: 1325
ISSN: 0021-9673
Sınıflandırma :
6
Ionic liquid intercalated clay sorbents for micro solid phase extraction of steroid hormones from water samples with analysis by liquid chromatography-tandem mass spectrometry
Dergi Makalesi

Dergi Makalesi
Kaynak :
DSpace Makaleler
Yayıncı :
Journal of Chromatography A
Yazar(lar) :
Aftafa Can , Pelit Fusun Okcu , Yalcinkaya Esra Evrim , Turkmen Hayati , Kapdan Ilgi , Ertas F. Nil
Konu :
Ionic liquids, Montmorillonite, Solid phase extraction, Endocrine disruptors, Estrogenic hormones, LC-MSMS
Yıl :
2014
Journal of Chromatography A
Yayıncı Web Sitesi
Kaydet
Clay material plays an important role in the transport and retention of many compounds in the soil, therefore, clay based sorbents are promising alternatives for selective sorption of organic pollutants. In the present work, different chain length ionic liquids (ILs) namely, 1-methyl-3-octyl-imidazolium bromide, 1-methyl-3-undecyl-imidazolium bromide and 1-methyl-3-octadecyl-imidazolium bromide were intercalated in the galleries of montmorillonite (MMT) clay. Then, this novel nanofiller surface was utilized in micro extraction of estrogenic hormones for the first time. A fast procedure where sonication-assisted emulsification microextraction combined with vortex assisted micro-solid phase extraction (mu-SPE) was developed for the LC-MS/MS analysis of estrone (E1), 17 beta-estradiol (E2), estriol (E3) and ethynylestradiol (EE2). The parameters related to the mu-SPE procedure namely; pH, sorbent amount, extraction solvent type and volume, sonication and vortex time, sample volume and salt effect on the extraction efficiency were screened by applying Plackett-Burmann design. The selected parameters were then optimized by using Box-Behnken design. The method was validated for the determination of estrogenic hormone residues in river water samples. Linear calibration plots were obtained for all hormones whose regression coefficients were larger than 0.98. RSD values were found less than 10% for three levels of concentration. LOD levels were calculated as; 0.012, 0.062, 0.018 and 0.693 ng L-1 for E1, E2, E3 and EE2, respectively. Recovery values were calculated in the range of 86.9-97.7%. Considering large sample volumes required for attaining low limits of these hormones, present method provides an ease for analyst as 10 mL of the sample is adequate for achieving the same sensitivity. (C) 2014 Elsevier B.V. All rights reserved.
Anahtar Kelimeler : Ionic liquids, Montmorillonite, Solid phase extraction, Endocrine disruptors, Estrogenic hormones, LC-MSMS, article
Cilt: 1361
ISSN: 0021-9673
Sınıflandırma :
Kimya %100
Kromatografi %100
7
Gas chromatographic-mass spectrometric analysis of essential oils from Pimpinella aurea, Pimpinella corymbosa, Pimpinella peregrina and Pimpinella puberula gathered from Eastern and Southern Turkey
Dergi Makalesi

Dergi Makalesi
Kaynak :
DSpace Makaleler
Yayıncı :
Journal of Chromatography A
Yazar(lar) :
Tabanca N , Demirci B , Kirimer N , Baser KHC , Bedir E , Khan IA , Wedge DE
Konu :
Pimpinella aurea, Pimpinella corymbosa, Pimpinella peregrina, Pimpinella puberula, essential oils, GC, GC-MS, phenylpropanoids, sesquiterpenes, monoterpenes
Yıl :
2005
Journal of Chromatography A
Yayıncı Web Sitesi
Kaydet
Essential oils from fruits, stems and leaves and roots of Pimpinella aurea DC., P. corymbosa Boiss., P. peregrina L. were analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) techniques. Fruits and aerial parts of P. puberula (DC.) Boiss were also evaluated. A total of 140 different compounds were identified, and significant qualitative and quantitative differences were observed among the samples. In fact, the main constituents of each species were different and only the oils extracted from roots shared the same principal compound, epoxy pseudoisoeugenyl-2-methyl butyrate (26.8-42.8%). The other fractions were dominated by different sesquiterpene compounds although in three of them, P. aurea stem and leaves, P. puberula fruits and P. puberula stems and leaves, monoterpene constituents also appear as main ones. (c) 2005 Elsevier B.V. All rights reserved.
Anahtar Kelimeler : Pimpinella aurea, Pimpinella corymbosa, Pimpinella peregrina, Pimpinella puberula, essential oils, GC, GC-MS, phenylpropanoids, sesquiterpenes, monoterpenes, article
Cilt: 1097
Sayı: 01.Feb
ISSN: 0021-9673
Sınıflandırma :
8
Gas chromatographic-mass spectrometric analysis of essential oils from Pimpinella species gathered from Central and Northern Turkey
Dergi Makalesi

Dergi Makalesi
Kaynak :
DSpace Makaleler
Yayıncı :
Journal of Chromatography A
Yazar(lar) :
Tabanca N , Demirci B , Ozek T , Kirimer N , Baser KHC , Bedir E , Khan IA , Wedge DE
Konu :
Pimpinella anisetum, Pimpinella anisum, Pimpinella affinis, Pimpinella cappadocica var. cappodocica, Pimpinella flabellifolia, Pimpinella isaurica, Pimpinella kotschyana, Pimpinella nudicaulis, Pimpinella olivieroides, Pimpinella peucedanifolia, Pimpinella rhodantha, Pimpinella saxifraga, Pimpinella tragium ssp lithophila, Pimpinella tragium ssp polyclada, Pimpinella tragium ssp pseudotragium, monoterpenes, sesquiterpenes, trinorsesquiterpens, phenylpropanoids
Yıl :
2006
Journal of Chromatography A
Yayıncı Web Sitesi
Kaydet
Essential oils from 15 Pimpinella species were analyzed by gas chromatography (GC) and gas chromatography-mass spectrometry (GC-MS) techniques. One species, Pimpinella anisum, in which only fruits were evaluated, was also included in the study. A total of 140 different compounds were identified and significant qualitative and quantitative differences were observed among the samples. Pimpinella essential oils were characterized as having mono-, sesqui- and trinorsesquiterpenoids, propenylphenols, and pseudoisoeugenols. Trinorsesquiterpenoids and phenylpropanoids appear to be chemical markers of Pimpinella species analyzed thus far. Essential oils obtained from Pimpinella roots share the same principal compound, epoxypseudoisoeugenyl-2-methylbutyrate at concentrations from 20 to 82.6%. (c) 2006 Elsevier B.V. All rights reserved.
Anahtar Kelimeler : Pimpinella anisetum, Pimpinella anisum, Pimpinella affinis, Pimpinella cappadocica var. cappodocica, Pimpinella flabellifolia, Pimpinella isaurica, Pimpinella kotschyana, Pimpinella nudicaulis, Pimpinella olivieroides, Pimpinella peucedanifolia, Pimpinella rhodantha, Pimpinella saxifraga, Pimpinella tragium ssp lithophila, Pimpinella tragium ssp polyclada, Pimpinella tragium ssp pseudotragium, monoterpenes, sesquiterpenes, trinorsesquiterpens, phenylpropanoids, article
Cilt: 1117
Sayı: 2
ISSN: 0021-9673
Sınıflandırma :
9
O-carboxymethyl chitosan Schiff base complexes as affinity ligands for immobilized metal-ion affinity chromatography of lysozyme
Dergi Makalesi

Dergi Makalesi
Kaynak :
DSpace Makaleler
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
Ömür Acet , Talat Baran , Demet Erdönmez , Neşe Hayat Aksoy , İhsan Alacabey , Ayfer Menteş , Mehmet Odabaşı
Konu :
Cryogel, IMAC, Carboxymethyl Chitosan, Lysozyme Adsorption
Yıl :
2018
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi
Kaydet
We synthesized Ni2+-attached O-Carboxymethyl chitosan Schiff base complexes embedded composite cryogels (Ni2+-O-CMCS-CCs) by means of polymerization of gel-forming precursors at subzero temperatures. Prepared affinity cryogel showed excellent adsorption performance for lysozyme selected as model protein to test adsorption parameters, demonstrating an adsorption capacity of 244.6 mg/g (15.3 mg/g for Ni2+ minus O-CMCS-CCs), with fast adsorption equilibrium within 30 min and good reversibility. The performance of Ni2+-O-CMCS-CCs for lysozyme was also evaluated by SDS-PAGE, and a purification efficiency of 86.9% with 89.5% purification yield was determined. The swelling test, FT-IR, and SEM analysis were carried out for the characterization of Ni2+-O-CMCS-CCs. At the end of 35 adsorption-desorption cycles, there was no significant change in the adsorption capacity.
Anahtar Kelimeler : Cryogel, IMAC, Carboxymethyl Chitosan, Lysozyme Adsorption, article
Cilt: 1550
ISSN: 0021-9673
Sınıflandırma :
10
Simultaneous determination of aliphatic and aromatic amines in water and sediment samples by ion-pair extraction and gas chromatography-mass spectrometry
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Dergi Makalesi
Kaynak 1:
DSpace Makaleler
Kaynak 2:
DSpace Makaleler
Yayıncı :
Journal of Chromatography A
Yazar(lar) :
Zonguldak Bülent Ecevit Üniversitesi
Konu :
Aliphatic, aromatic amines, Environmental water, sediment samples, GC-MS, Ion-pair extraction
Yıl :
2006
Journal of Chromatography A
Piri Tam Metin Bulucu
Kaydet
A gas chromatography-mass spectrometry (GC-MS) method has been proposed for the determination of aliphatic and aromatic amines in a variety of environmental samples including wastewater, river water, sea water and sediment samples. The method includes ion-pair extraction with bis-2-ethylhexylphosphate (BEHPA), derivatisation of compounds with isobutyl chloroformate (IBCF) and their GC-MS analysis. Aliphatic and aromatic amines were isolated from aqueous samples using BEHPA as ion-pair reagent and derivatised with IBCF for their chromatographic analysis. Solid-liquid extraction of aliphatic and aromatic amines in sediment samples were performed in Soxhlet apparatus with acidic MeOH and ion-pair extraction with BEHPA were carried out for the isolation of amines followed by derivatisation with IBCF. Aliphatic and aromatic amines were then analysed with GC-MS in both electron impact (EI) and positive and negative ion chemical ionisation (PNICI) mode as their isobutyloxycarbonyl (isoBOC) derivatives. The obtained recoveries ranged from 81.0 to 98.0% and the precision of this method, as indicated by the relative standard deviations (RSDs) was within the range of 0.5 and 4.3%. The detection limits obtained from calculations by using GC-MS results based on S/N = 3 were within the range from 0.07 to 0.50 ng/l. © 2006 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2006.06.075
Anahtar Kelimeler : Aliphatic and aromatic amines, Environmental water and sediment samples, GC-MS, Ion-pair extraction, article
Cilt: 1129
Sayı: 1
ISSN: 0021-9673
Sınıflandırma :
Kimya %100
Kromatografi %100
11
Determination of trans-10-hydroxy-2-decenoic acid content in pure royal jelly and royal jelly products by column liquid chromatography
Dergi Makalesi

Dergi Makalesi
Kaynak :
DSpace Makaleler
Yayıncı :
Journal of Chromatography A
Yazar(lar) :
Genc M , Aslan A
Konu :
royal jelly, trans-10-hydroxy-2-decenoic acid
Yıl :
1999
Journal of Chromatography A
Yayıncı Web Sitesi
Kaydet
In this research, several royal jellies and commercial products containing royal jelly were analysed for their trans-10-hydroxy-2-decenoic acid (10-HDA) content by using a column liquid chromatography technique. Ten samples claimed to be pure royal jelly, containing 10-HDA between 0.75 and 2.54%. Seven samples claimed to contain royal jelly as an ingredient which ranged from non-detectable to 0.054%. The technique was found to be rapid with high recovery. (C) 1999 Elsevier Science B.V. All rights reserved.
Anahtar Kelimeler : royal jelly, trans-10-hydroxy-2-decenoic acid, article
Cilt: 839
Sayı: 01.Feb
ISSN: 0021-9673
Sınıflandırma :
12
Dye-ligand and metal chelate poly(2-hydroxyethylmethacrylate) membranes for affinity separation of proteins
Dergi Makalesi

Dergi Makalesi
Kaynak :
DSpace Makaleler
Yayıncı :
Journal Of Chromatography A
Yazar(lar) :
MY Arica , HN Testereci , A Denizli
Konu :
affinity membranes, membranes, metal chelate affinity chromatography, poly(2-hydroxyethyl methacrylate) membranes, affinity adsorbents, proteins, enzymes, metal chelates, iron, cibacron blue F3GA
Yıl :
1998
Journal Of Chromatography A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
Cibacron Blue F3GA was covalently immobilized onto poly(2-hydroxyethyl methacrylate) (pHEMA) membranes via the nucleophilic reaction between the chloride of its triazine ring and the hydroxyl group of pHEMA. Then, Fe3+ ions were complexed by chelation with the immobilized Cibacron Blue F3GA molecules. Different amounts of Fe3+ ions were loaded on the membranes by changing the concentration of Fe3+ ions and pH of the reaction medium. Membranes with or without Fe3+ were used in the adsorption of glucose oxidase, catalase and bovine serum albumin. The adsorption capacities of these membranes were determined by changing pH and the concentration of the proteins in the adsorption medium. The adsorption phenomena appeared to follow a typical Langmuir isotherm. The maximum capacities (q(m)) of the Fe3+ complexed membranes for glucose oxidase, catalase and bovine serum albumin (8.70.10(-3) mu mol m(-2), 2.15.10(-3) mu mol m(-3) and 2.21.10(-3) mu mol m(-2)) were greater than those of the untreated membranes (6.79.10(-3) mu mol m(-2), 1.34.10(-3) mu mol m(-2) and 1.94.10(-3) mu mol m(-2)) respectively. The nonspecific adsorption of the enzymes and the protein on the pHEMA membranes was negligible. (C) 1998 Elsevier Science B.V.
DOI : 10.1016/S0021-9673(97)01079-0
Anahtar Kelimeler : affinity membranes, membranes, metal chelate affinity chromatography, poly(2-hydroxyethyl methacrylate) membranes, affinity adsorbents, proteins, enzymes, metal chelates, iron, cibacron blue F3GA, article
Cilt: 799
Sayı: 1-2
ISSN: 0021-9673
Sınıflandırma :
Kimya %100
Nanokimya %47
13
Cibacron Blue F3GA-incorporated macroporous poly(2-hydroxyethyl methacrylate) affinity membranes for heavy metal removal
Dergi Makalesi

Dergi Makalesi
Kaynak :
DSpace Makaleler
Yayıncı :
Journal Of Chromatography A
Yazar(lar) :
A Denizli , B Salih , MY Arica , K Kesenci , V Hasirci , E Piskin
Konu :
affinity membranes, adsorption, Cibacron Blue, poly(2-hydroxyethyl methacrylate), metals, arsenic, cadmium, lead
Yıl :
1997
Journal Of Chromatography A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
Macroporous poly(2-hydroxyethyl methacrylate), poly(HEMA), membranes were prepared by UV-initiated photo-polymerization of HEMA in the presence of an initiator (azobisisobutyronitrile, AIBN). An affinity dye, i.e., Cibacron Blue F3GA was then incorporated covalently. These affinity membranes with a swelling ratio of 58%, and carrying 10.67 mmol Cibacron Blue F3GA/m(2) membrane were used in the adsorption/desorption of some selected heavy metal ions [i.e., As(III), Cd(II) and Pb(II)] from aqueous media. Very high adsorption rates were observed and adsorption equilibria were reached in about 30 min. The maximum adsorptions of heavy metal ions onto the dye-incorporated affinity membranes from their single solutions were 12.6 mmol/m(2) for As(III), 61.0 mol/m(2) for Cd(II) and 79.0 mol/m(2) for Pb(II), However, when the heavy metal ions competed (in the case of the adsorption from their mixture) the amounts of adsorption for As(III), Cd(II) and Pb(II) were quite close. Desorption of heavy metal ions was carried out by using 0.1 M HNO3 (pH 1.0). Up to 95% of the adsorbed heavy metal ions were desorbed in 60 min. Repeated adsorption/desorption cycles showed the feasibility of this novel affinity membrane for heavy metal removal.
DOI : 10.1016/S0021-9673(96)00725-X
Anahtar Kelimeler : affinity membranes, adsorption, Cibacron Blue, poly(2-hydroxyethyl methacrylate), metals, arsenic, cadmium, lead, article
Cilt: 758
Sayı: 2
ISSN: 0021-9673
Sınıflandırma :
Kimya %73
Nanokimya %91
14
Monolithic stationary phases with incorporated fumed silica nanoparticles. Part II. Polymethacrylate-based monolithic column with covalently incorporated modified octadecyl fumed silica nanoparticles for reversed-phase chromatography
Araştırma Makalesi

Araştırma Makalesi Open Access
Kaynak :
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
Ziad El Rassi , Cemil Aydogan
Yıl :
2016
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
This study is concerned with the incorporation of surface modified fumed silica nanoparticles (FSNPs) into polymethacrylate based monolithic columns for use in reversed phase chromatography (RPC) of small solutes and proteins. First, FSNPs were modified with 3-(trimethoxysilyl)propylmethacrylate (TMSPM) to yield the hybrid methacryloyl fumed silica nanoparticle (MFSNP) monomer. The resulting MFSNP was then mixed with glyceryl monomethacrylate (GMM) and ethylene dimethacrylate (EDMA) in a binary porogenic solvent composed of cyclohexanol and dodecanol, and the in situ copolymerization of MFSNP, GMM and EDMA was performed in a stainless steel column of 4.6 mm i.d. The silanol groups of the hybrid monolith thus obtained were grafted with octadecyl ligands by perfusing the hybrid monolithic column with a solution of 4% w/v of dimethyloctadecylchlorosilane (DODCS) in toluene while the column was maintained at 110 degrees C for 6 h (in a heated HPLC oven). One of the originalities of this study was to demonstrate MFSNP as a novel derivatized hybrid monomer in making RPC monolithic columns with surface bound octadecyl ligands. In this respect, the RPC behavior of the monolithic column with covalently incorporated FNSPs having surface grafted octadecyl ligands was evaluated with alkylbenzenes, aniline derivatives and phenolic compounds. The results showed that the hybrid poly(GMA-EDMA-MFSNP) having surface bound octadecyl ligands exhibited hydrophobic interactions under reversed phase elution conditions. Furthermore, six standard proteins were baseline separated on the column using a 10 min linear gradient elution at increasing ACN concentration in the mobile phase at a flow rate of 1.0 mL/min using a 10 cm x 4.6 mm i.d. column. The relative standard deviations (RSDs) for the retention times of the tested solutes were lower than 2.1% and 2.4% under isocratic elution and gradient elution conditions, respectively. (C) 2016 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2016.03.083
Sayi :1445
Sayfa :62-67
Sınıflandırma :
Kimya %100
Kromatografi %100
15
Improved and simplified liquid chromatography/atmospheric pressure chemical ionization mass spectrometry method for the analysis of underivatized free amino acids in various foods
Araştırma Makalesi

Araştırma Makalesi Open Access
Kaynak :
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
Hamide Z Senyuva , Sureyya Ozcan
Yıl :
2006
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
An improved analytical method which offers rapid, accurate determination and identification of 22 amino acids in a variety of matrices, e.g. baby foods, juices, honey is reported. The amino acids were extracted from the matrixes using acidified water. Simultaneous determination of 22 underivatized amino acids was carried out by a liquid chromatography-mass spectrometry (LC/MS). A narrow-bore column allowed rapid screening and quantitative analysis by positive LC/atmospheric pressure chemical ionization (APCI) MS with only acidified mobile phase. Retention times of the 22 amino acids were in the range of ca. 0.9-7.5 min. Sample preparation without clean-up followed by fast chromatographic analysis allowed the analysis to be completed in < 25 min. (c) 2006 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2006.09.039
Sayi :1135
issue :2
Sayfa :179-185
Sınıflandırma :
Kimya %100
Kromatografi %100
16
Synthesis of a reactive polymethacrylate capillary monolith and its use as a starting material for the preparation of a stationary phase for hydrophilic interaction chromatography
Araştırma Makalesi

Araştırma Makalesi Open Access
Kaynak :
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
Ali Tuncel , Bekir Celebi , Aslihan Gokaltun , Damla Erkakan , Cigdem Kip
Yıl :
2015
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
Poly(3-chloro-2-hydroxypropyl methacrylate-co-ethylene dimethacrylate), poly(HPMA-Cl-co-EDMA) capillary monolith was proposed as a reactive starting material with tailoring flexibility for the preparation of monolithic stationary phases. The reactive capillary monolith was synthesized by free radical copolymerization of 3-chloro-2-hydroxypropyl methacrylate (HPMA-Cl) and ethylene dimethacrylate (EDMA). The mean pore size, the specific surface area and the permeability of poly(HPMA-Cl-co-EDMA) monoliths were controlled by adjusting porogen/monomer volume ratio, porogen composition and polymerization temperature. The porogen/monomer volume ratio was found as the most effective factor controlling the porous properties of poly(HPMA-Cl-co-EDMA) monolith. Triethanolamine (TEA-OH) functionalized polymethacrylate monoliths were prepared by using the reactive chloropropyl group of poly(HPMA-Cl-co-EDMA) monolith via one-pot and simple post-functionalization process. Poly(HPMA-Cl-co-EDMA) monolith reacted with TEA-OH was evaluated as a stationary phase in nano-hydrophilic interaction chromatography (nano-HILIC). Nucleotides, nucleosides and benzoic acid derivatives were satisfactorily separated with the plate heights up to 20 mu m. TEA-OH attached-poly(HPMA-Cl-co-EDIVIA) monolith showed a reproducible and stable retention behaviour in nano-HILIC runs. However, a decrease in the column performance (i.e. an increase in the plate height) was observed with the increasing retention factor. Hence retention-dependent column efficiency behaviour was shown for HILIC mode using the chromatographic data collected with the polymer based monolith synthesized. (C) 2015 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2015.04.005
Sayi :1396
Sayfa :86-97
Sınıflandırma :
Kimya %100
Kromatografi %100
17
The role of the acquisition methods in the analysis of natural and synthetic steroids and cholic acids by gas chromatography-mass spectrometry
Araştırma Makalesi

Araştırma Makalesi Open Access
Kaynak :
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
I Molnar-Perl , Gy Zaray , A Vasanits-Zsigrai , A Helenkar , N Andrasi
Yıl :
2011
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
An exhaustive GC-MS acquisition study was performed, for the simultaneous analysis of natural and synthetic steroids and cholic acids (in order to insert them into the last tierce of our multiresidue analysis system), such as androsterone, beta-estradiol, transdehydroandro-sterone. transdehyroandrosterone, mestranol, dihydrotestosterone, ethinylestradiol, testosterone, norethisterone, estriol, 4-androstene-3,17-dione, gestodene, levonorgestrel, etonogestrel, coprostanol, progesterone, cholesterol, medroxyprogesterone-acetate, lithocholic acid, stigmasterol, cholic acid, chenodeoxycholic acid, beta-sitosterol, ursodeoxycholic acid, 3-hydroxy-7-ketocholic acid and dehydrocholic acid, in total 26 compounds. As novelties to the field, for the trimethylsilyl (TMS) oxime ether/ester derivatives of steroids and cholic acids, at first, a tandem mass spectrometric (MS/MS), multiple reaction monitoring (MRM) type acquisition method has been developed in a single run; also for the first time, the three acquisition techniques, the full scan (FS), the selective ion monitoring (SIM), in our case the multiple ion monitoring (MIM) and the currently optimized MRM methods, have been compared; all three, in parallel, under strictly the same derivatization/instrumental conditions, both in matrix free solutions and municipal wastewater from two Hungarian wastewater treatment plants (WWTPs). Critical evaluation of the three acquisition protocols was collated on their analytical performances and validated under the same conditions. The data of six point calibration curves for FS, MIM and MRM methods, showed that both R(2) (0.9995, 0.9858, 0.9975) and RSD (5.3, 5.8, 5.0), for two parallel derivatizations, each injected three times, proved to be independent of the acquisition processes. Whereas, for the method limit of quantification (LOQ) and the instrument limit of quantification (ILQ) values showed considerable differences. LOQ data, were decreasing in the FS, MIM, MRM line (expressed in ng/L), for all steroids and cholic acids. The same trend was determined in terms of the ILQ values. The practical utility of the optimized acquisition techniques was confirmed by the quantitation of the steroids and cholic acids contents of wastewater samples. Results confirmed the importance of the MRM acquisition method, even in comparison to the MIM one: with particular interest in selected cases: avoiding the extreme overestimation of the beta-estradiol (156-1325%) and that of the ethinylestradiol (582-831%) concentrations in the wastewater samples. (C) 2011 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2011.09.006
Sayi :1218
issue :45
Sayfa :8264-8272
Sınıflandırma :
Kimya %100
Kromatografi %95
18
Derivatization and fragmentation pattern analysis of natural and synthetic steroids, as their trimethylsilyl (oxime) ether derivatives by gas chromatography mass spectrometry: Analysis of dissolved steroids in wastewater samples
Araştırma Makalesi

Araştırma Makalesi Open Access
Kaynak :
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
I Molnar-Perl , A Vasanits , Gy Zaray , A Helenkar , N Andrasi
Yıl :
2011
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
This paper reports the extension of our multiresidue analysis (MA) procedure with 18 natural and synthetic steroids; permitting the identification and quantification, in total of 81 pollutants from one solution, by a single injection, as their trimethylsilyl (TMS)-oxime ether/ester derivatives, by gas chromatography-mass spectrometry (GC-MS), within 31 min. As a novelty to the field, basic researches, such as fragmentation pattern analysis and derivatization optimization studies were performed for androsterone, transdehydroandrosterone, transandrosterone, mestranol, dihydrotestosterone, ethinylestradiol, testosterone, norethisterone, estriol, 4-androstene-3,17-dione, gestodene, levonorgestrel, etonogestrel, coprostanol, progesterone, cholesterol, medroxy-progesterone-acetate, stigmasterol and beta-sitosterol. Results confirmed that (i) the TMS oxime-ether derivatives of the keto steroids provide from 1.40 times (gestodene) up to 4.25 times (norethisterone) higher responses compared to their TMS-ether ones, and (ii) the distribution of syn/anti oximes is characteristic to the ketosteroid species examined. Based on our optimized mass fragmentation, solid phase extraction (SPE) and derivatization studies separations have been performed in the total ion current (TIC) mode, identification and quantification of compounds have been carried out on the basis of their selective fragment ions. Responses, obtained with derivatized standards proved to be linear (hydroxysteroids), or have been calculated from calibration curves (ketosteroids) in the range of 1.88-750 ng/L levels. Limit of quantitation (LOQ) values varied between 1.88 ng/L and 37.5 ng/L concentrations. The most important practical messages of this work are the high androsterone (0.744-4.28 mu g/L), transandrosterone (0.138-4.00 mu g/L). coprostanol (2.11-302 mu g/L), cholesterol (0.308-41 mu g/L), stigmasterol (1.21-8.40 mu g/L)and beta-sitosterol (1.12-11.0 mu g/L) contents of influent wastewaters. beta-Estradiol (100 ng/L) and estriol (54 ng/L) were found in one influent sample, only. Reproducibilities, characterized with the relative standard deviation percentages (RSD%) of measurements, varied between 1.73 RSD% (beta-estradiol) and 5.4 RSD% (stigmasterol), with an average of 4.82 RSD%. (C) 2011 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2011.01.051
Sayi :1218
issue :14
Sayfa :1878-1890
Sınıflandırma :
Kimya %100
Kromatografi %100
19
Simple high-performance liquid chromatographic method for determination of atropine and obidoxime in a parenteral injection device
Araştırma Makalesi

Araştırma Makalesi Open Access
Kaynak :
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
D Karakas , S Yenisoy-Karakas , M Bilsel , G Bilsel , AC Goren
Yıl :
2004
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
Atropine and obidoxime in a parenteral injection device are determined by simple HPLC method simultaneously without any pretreatment at 228 nm. The relative standard deviations (R.S.D.) were below 1.6% for the compounds. The correlation coefficient was greater than 0.999 for both compounds in the calibration range. The recoveries at 5 mg/L concentration averaged as 95% for atropine and 102% for obidoxime. The uncertainty of the measurements for atropine and obidoxime was 2.8% and 2.4%, respectively. (C) 2004 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2004.09.048
Sayi :1057
issue :1-2
Sayfa :237-239
Sınıflandırma :
Kimya %98
Kromatografi %100
20
Determination of Ochratoxin A traces in foodstuffs: Comparison of an automated on-line two-dimensional high-performance liquid chromatography and off-line immunoaffinity-high-performance liquid chromatography system
Araştırma Makalesi

Araştırma Makalesi Open Access
Kaynak :
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
Adil Denizli , Lokman Uzun , Canan Armutcu
Yıl :
2018
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
Automated on-line two-dimensional high-performance liquid chromatography method (2D-HPLC) is proposed to determine Ochratoxin A (OTA) in food samples as an alternative to OTA immunoaffinity column (IAC). An on-line 2D-HPLC system is designed for the analysis of OTA using an affinity-based monolithic column in the first dimension and reversed-phase C18 column in the second dimension. Initially, optimal OTA separation efficiency is determined through traditional HPLC system consisting of a P(HEMAPA) monolithic column coupled with HPLC system. Secondly, after providing optimum conditions, OTA determination was investigated through the 2D-HPLC system. According to results, 2D-HPLC system showed good linearity in the range 0.5 to 20 ng/mL with limit of detection (LOD) and limit of quantification (LOQ) values of 21.2 pg/mL and 64.3 pg/mL, respectively. The P(HEMAPA)-4 monolithic column displayed good recovery of OTA ranging from 104.34% to 107.33%. Relative standard deviations (RSD) varied in the range 0.21% to 1.31% thus indicating the efficiency of P(HEMAPA)-4 monolithic column developed for OTA. (C) 2018 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2018.07.057
Sayi :1569
Sayfa :139-148
Sınıflandırma :
Kimya %100
Kromatografi %100
21
A rapid and simple method for simultaneous determination of triphenylmethane dye residues in rainbow trouts by liquid chromatography-tandem mass spectrometry
Araştırma Makalesi

Araştırma Makalesi Open Access
Kaynak :
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
Oznur Karaoglu , Elmas O Olgun , Muammer Kaplan
Yıl :
2014
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
A rapid and simple LC-MS/MS method was developed and optimized for screening and confirmation of triphenylmethane dyes including malachite green (MG), leucomalachite green (LMG), crystal violet (CV), leucocrystal violet (LCV) and brilliant green (BG) in fish muscle with skin. Leucocrystal violet D6 (LCV-D6) and leucomalachite green-D5 (LMG D5) was used as internal standards. Sample preparation is a simple procedure based on solid-liquid extraction with acetonitrile containing 1% acetic acid, followed by centrifugation and evaporation of the supernatant. The residue was dissolved in acetonitrile with 0.1% acetic acid and centrifuged prior to LC-MS/MS analysis. Chromatographic separation of analytes was performed on an Inertsil ODS-4 C18 column with ammonium acetate buffer in acetonitrile gradient. The mass detection was performed on a triple-quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) mode via electrospray ionization (ESI+). The developed method was validated according to the criteria set in Commission Decision 2002/657/EC. The decision limit (CC alpha) was 0.43, 0.24, 0.33, 0.28 and 0.17 mu g kg(-1) for MG, LMG, CV, LCV and BG respectively. The detection capability (CC beta) values obtained were 0.56, 0.31, 0.43, 0.37 and 0.22 mu g kg(-1), respectively. The precision of the method, expressed as relative standard deviation (RSD) values for the within-day and inter-day laboratory reproducibility, for MG, LMG, CV, LCV and BG at the four levels of fortification (0.3, 0.5, 1, and 2 mu g kg(-1)), was less than 16 and 19% respectively. Accuracy of the method was confirmed by successful participation of a proficiency test organized by FAPAS. The method has been used for the analysis of 208 fish samples of which seven samples were found to be non-compliant containing low residues of LMG and LCV. (C) 2014 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2014.04.091
Sayi :1349
Sayfa :37-43
Sınıflandırma :
Kimya %100
Kromatografi %100
22
Determination of acrylamide in potato chips and crisps by high-performance liquid chromatography
Araştırma Makalesi

Araştırma Makalesi Open Access
Kaynak :
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
K Sarioglu , J Acar , HZ Senyuva , V Gokmen
Yıl :
2005
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
A simple and rapid method using liquid chromatography coupled to diode array detection (LC-DAD) was developed for the determination of acrylamide in potato-based foods at low levels. The method entails extraction of acrylamide with methanol, purification with Carrez I and 11 solutions, evaporation and solvent change to water, and cleanup with a Oasis HLB solid-phase extraction (SPE) cartridge. The final extract was analyzed by LC-DAD for quantification and by liquid chromatography coupled to mass spectrometry (LC-MS) for confirmation. The chromatographic separations were performed on a hydrophilic and a hydrophobic interaction columns having good retention of acrylamide under 100% aqueous flow conditions (k 3.67 and 2.54, respectively). The limit of quantitation was estimated to be 4.0 mu g/kg based on the signal-to-noise ratio of 3 recorded at 226 nm. Recoveries of acrylamide from potato chips samples spiked at levels of 250, 500 and 1000 (n = 4 for each level) mu g/kg ranged between 92.8 and 96.2% with relative standard deviations of less than 5%. The results of this study revealed that a conventional LC instrument coupled to DAD can also be used accurately and precisely, as an alternative to tandem LC-MS methods for the determination of acrylamide in potato-based foods. (c) 2004 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2004.10.094
Sayi :1088
issue :1-2
Sayfa :193-199
Sınıflandırma :
Kimya %100
Kromatografi %100
23
A generic method for the determination of acrylamide in thermally processed foods
Araştırma Makalesi

Araştırma Makalesi Open Access
Kaynak :
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
Hamide Z Senyuva , Vural Gokmen
Yıl :
2006
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
A generic sample preparation method for the determination of acrylamide in foods was developed. The method entails extraction with methanol, purification with Carrez I and II solutions, evaporation and solvent change to water, and cleanup with Oasis HLB solid-phase extraction (SPE) cartridge. The final extract was analyzed by liquid chromatography-mass spectrometry (LC-MS) for quantitation. The chromatographic separation was performed on ODS-3 column using the isocratic mixture of 0.01 mM acetic acid in 0.2% aqueous solution of formic acid at a flow rate of 0.6 ml/min at 25 degrees C. The recoveries of acrylamide from potato chips, biscuits and coffee ranged between 92.8 and 101.5% with relative standard deviations of 4.1% or less. The limit of detection (LOD) and the limit of quantitation (LOQ) were 2 ng/g and 6 ng/g in the basis of signal to noise ratios of 3: 1 and 9: 1, respectively. (c) 2006 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2006.01.084
Sayi :1120
issue :1-2
Sayfa :194-198
Sınıflandırma :
Kimya %100
Kromatografi %100
24
Monolithic stationary phases with incorporated fumed silica nanoparticles. Part I. Polymethacrylate-based monolithic column with incorporated bare fumed silica nanoparticles for hydrophilic interaction liquid chromatography
Araştırma Makalesi

Araştırma Makalesi Open Access
Kaynak :
Aperta - TÜBİTAK Açık Arşivi
Yayıncı :
JOURNAL OF CHROMATOGRAPHY A
Yazar(lar) :
Ziad El Rassi , Cemil Aydogan
Yıl :
2016
JOURNAL OF CHROMATOGRAPHY A
Yayıncı Web Sitesi Piri Tam Metin Bulucu
Kaydet
Fumed silica nanoparticles (FSNPs), were incorporated for the first time into a polymethacrylate monolithic column containing glyceryl monomethacrylate (GMM) and ethylene dimethacrylate (EDMA) in order to develop a new monolithic column for hydrophilic interaction high performance liquid chromatography (HILIC). When compared to poly(GMM-EDMA) monolithic column without FSNPs, the same monolithic column with incorporated FSNPs yielded important effects on HILIC separations. The effects of monomers and FSNPs content of the polymerization mixture on the performance of the monolithic column were examined in details, and the optimized stationary phase was investigated over a wide range of mobile phase composition with polar acidic, weakly basic and neutral analytes including hydroxy benzoic acids, nucleotides, nucleosides, dimethylformamide, formamide and thiourea. The retention of these analytes was mainly controlled by hydrophilic interactions with the FSNPs and electrostatic repulsion from the negatively charged silica surface in the case of hydroxy benzoic acids and nucleotides. The electrostatic repulsion was minimized by decreasing the pH of the aqueous component of the mobile phase, which in turn enhanced the retention of acidic solutes. Nucleotides were best separated using step gradient elution at decreasing pH as well as ACN concentration in the mobile phase. Improved peak shape and faster analysis of nucleosides were attained by a fast linear gradient elution with a shallow decrease in the ACN content of the ACN-rich mobile phase. The run-to-run and column-to-column reproducibility were satisfactory. The percent relative standard deviations (%RSDs) for the retention times of tested solutes were lower than 2.5% under isocratic conditions and lower than 3.5 under gradient conditions. (C) 2016 Elsevier B.V. All rights reserved.
DOI : 10.1016/j.chroma.2016.03.075
Sayi :1445
Sayfa :55-61
Sınıflandırma :
Kimya %100
Kromatografi %100
25
Therapeutic drug monitoring for sirolimus in whole blood of organ transplants by high-performance liquid chromatography with ultraviolet detection
Araştırma Makalesi

Araştırma Makalesi
Kaynak :
Science Direct
Yayıncı :
Journal of Chromatography A
Yazar(lar) :
Miguel Angel Campanero , Ernesto Cardenas , Belén Sádaba , Emilio Garcı́a-Quetglas , Maria Jose Muñoz-Juarez , Isabel Gil-Aldea , David Pazo , Jose Ramón Azanza , Jesús Honorato
Yıl :
2004
Journal of Chromatography A
Yayıncı Web Sitesi Tam Metin
Kaydet
We developed and validated an accurate, sensitive, precise and rapid HPLC method with UV detection for the determination of sirolimus in blood samples from renal, cardiac and hepatic transplants. This method overcomes most of the problems related to previously published assays using a narrow-bore column with base deactivated C18 reversed phase. Whole blood samples were purified by a combination of a precipitating blood matrix with zinc sulphate and a single step liquid–liquid extraction with acetone and 1-chlorobutane. Calibration curves (range 2.5–150 ng/ml), were linear with coefficients of correlation better than 0.996. The relative standard deviation was determined to be less than 8%. The present method has also been validated by a reference laboratory (St. George’s Hospital Medical School, London, UK). More of 300 clinical samples have been analysed with this method.
DOI : 10.1016/j.chroma.2003.10.121
Anahtar Kelimeler : Validation, Sirolimus, Rapamycin, Lactones, Demethoxyrapamycin
Cilt: 1031
Sayı: 1-2
Sayfa: 265-273
ISSN: 0021-9673

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