Titanium-scaffolded organic-monolithic stationary phases for ultra-high-pressure liquid chromatography

Vonk, Rudy J.; Vaast, Axel; Eeltink, Sebastiaan; Schoenmakers, Peter J.

doi:10.1016/j.chroma.2014.07.039

Cited by 29 publications

(23 citation statements)

References 22 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…The unwanted effects of shrinking are negligible in capillaries, although very important in larger diameter tubes. A few approaches to reduce the shrinking effects have been suggested, including the use of solvents that keep the stationary phase in the swollen-state [9], polymerization under high pressures [10], and the employ of a titanium scaffold [11].…”

Section: Introductionmentioning

confidence: 99%

Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography

Catalá-Icardo

Torres-Cartas

Lloret

et al. 2017

Analytica Chimica Acta

View full text Add to dashboard Cite

In this work, a method for the preparation and anchoring of polymeric monoliths in a polytetrafluoroethylene (PTFE) tubing as a column housing for microbore HPLC is described. In order to assure a covalent attachment of the monolith to the inner wall of the PTFE tube, a two-step procedure was developed. Two surface etching reagents, a commercial sodium naphthalene solution (Fluoroetch), or mixtures of HO and HSO, were tried and compared. Then, the obtained hydroxyl groups on the PTFE surface were modified by methacryloylation. Attenuated total reflectance Fourier-transform infrared (ATR-FTIR) spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the tubing wall and the stable anchorage of monolith to the wall, respectively. Special emphasis was also put on the reduction of the unwanted effects of shrinking of monolith during polymerization, by using an external proper mold and by selecting the adequate monomers in order to increase the flexibility of the polymer. Poly(glycidyl methacrylate-co-divinylbenzene) monoliths were in situ synthesized by thermal polymerization within the confines of surface-vinylized PTFE tubes. The modified PTFE tubing tightly held the monolith, and the monolithic column exhibited good pressure resistance up to 20 MPa. The column performance was also evaluated via the isocratic separation of a series of alkylbenzenes in the reversed-phase mode. The optimized monolithic columns gave plate heights ranged between 70 and 80 μm. The resulting monoliths were also satisfactorily applied to the separation of proteins.

show abstract

Section: Introductionmentioning

confidence: 99%

Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography

Catalá-Icardo

Torres-Cartas

Lloret

et al. 2017

Analytica Chimica Acta

View full text Add to dashboard Cite

show abstract

“…After polymerization, the monolithic columns were thoroughly flushed with MeOH before analyses to remove all unreacted monomers and porogenic solvents. The preparation of the S- co -DVB monoliths in glass-lined tubing was described in detail in our previous work [ 24 ].…”

Section: Methodsmentioning

confidence: 99%

“…The “nano-scale” photografted columns (internal diameter 100 μm) were used in the first dimension ( 1 D) in combination with a “capillary scale” (internal diameter 0.8 mm) S- co -DVB column in the second dimension ( 2 D). For analyses of tryptic-digested cytochrome c , tryptic-digested bovine serum albumin (BSA) and tryptic-digested mixture of six proteins (PMD), the ion-exchange and reversed phase conditions were taken from literature [ 24 , 25 ] and adapted for online coupling of the two methods using a UV detector. Finally, the applicability of the SCX × RPLC setup was demonstrated with the analyses of a BSA digest by hyphenation to a high-resolution Fourier transform ion cyclotron resonance mass spectrometer (FTICR-MS).…”

Section: Introductionmentioning

confidence: 99%

Post-polymerization photografting on methacrylate-based monoliths for separation of intact proteins and protein digests with comprehensive two-dimensional liquid chromatography hyphenated with high-resolution mass spectrometry

et al. 2015

Self Cite

View full text Add to dashboard Cite

Post-polymerization photografting is a versatile tool to alter the surface chemistry of organic-based monoliths so as to obtain desired stationary phase properties. In this study, 2-acrylamido-2-methyl-1-propanesulfonic acid was grafted to a hydrophobic poly(butyl methacrylate-co-ethylene glycol dimethacrylate) monolith to create a strong cation exchange stationary phase. Both single-step and two-step photografting were addressed, and the effects of grafting conditions were assessed. An experimental design has been applied in an attempt to optimize three of the key parameters of the two-step photografting chemistry, i.e. the grafting time of the initiator, the monomer concentration and the monomer irradiation time. The photografted columns were implemented in a comprehensive two-dimensional column liquid chromatography (tLC × tLC) workflow and applied for the separation of intact proteins and peptides. A baseline separation of 11 intact proteins was obtained within 20 min by implementing a gradient across a limited RP composition window in the second dimension. tLC × tLC with UV detection was used for the separation of cytochrome c digest, bovine serum insulin digest and a digest of a complex protein mixture. A semi-quantitative estimation of the occupation of separation space, the orthogonality, of the tLC × tLC system yielded 75 %. The tLC × tLC setup was hyphenated to a high-resolution Fourier transform ion cyclotron resonance mass spectrometer instrument to identify the bovine serum insulin tryptic peptides and to demonstrate the compatibility with MS analysis.Electronic supplementary materialThe online version of this article (doi:10.1007/s00216-015-8615-4) contains supplementary material, which is available to authorized users.

show abstract

“…For instance, the monolith shrinkage during polymerization, albeit negligible in capillaries, it is strong enough to breakdown the monolith-tube anchorage when larger diameter tubes are employed. In this sense, certain strategies have been proposed, such as the use of an external mold together with a proper selection of monomers providing a highly flexible polymer [9], a titanium scaffold [10], solvents that keep the stationary phase in the swollen-state [11], and polymerization under high pressures [12].…”

Section: Introductionmentioning

confidence: 99%

Photografted fluoropolymers as novel chromatographic supports for polymeric monolithic stationary phases

Catalá-Icardo

Torres-Cartas

Lloret

et al. 2018

Talanta

View full text Add to dashboard Cite

In this study, porous polymer monoliths were in situ synthesized in fluoropolymers tubing to prepare microbore HPLC columns. To ensure the formation of robust homogeneous polymer monoliths in these housing supports, the inner surface of fluoropolymer tubing was modified in a two-step photografting process. Raman spectroscopy and scanning electron microscopy (SEM) confirmed the successful modification of the inner poly(ethylene-co-tetrafluoroethylene) (ETFE) wall and the subsequent attachment of a monolith onto the wall. Poly(glycidyl methacrylate-co-divinylbenzene), poly(butyl methacrylate-co-ethyleneglycol dimethacrylate) and poly(styrene-co-divinylbenzene) monoliths were in situ synthesized by thermal polymerization within the confines of surface vinylized ETFE tubes. The resulting monoliths exhibited good permeability and mechanical stability (pressure resistance up to 9 MPa). The chromatographic performance of these different monolithic columns was evaluated via the separation of alkyl benzenes and proteins in a conventional HPLC system.

show abstract

Titanium-scaffolded organic-monolithic stationary phases for ultra-high-pressure liquid chromatography

Cited by 29 publications

References 22 publications

Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography

Preparation of organic monolithic columns in polytetrafluoroethylene tubes for reversed-phase liquid chromatography

Post-polymerization photografting on methacrylate-based monoliths for separation of intact proteins and protein digests with comprehensive two-dimensional liquid chromatography hyphenated with high-resolution mass spectrometry

Photografted fluoropolymers as novel chromatographic supports for polymeric monolithic stationary phases

Contact Info

Product

Resources

About