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Method transfer from high-pressure liquid chromatography to ultra-high-pressure liquid chromatography. II. Temperature and pressure effects
Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper. (Interact)ORCID-id: 0000-0001-8561-6872
Karlstads universitet, Fakulteten för hälsa, natur- och teknikvetenskap (from 2013), Institutionen för ingenjörs- och kemivetenskaper. (Interact)ORCID-id: 0000-0003-1819-1709
Department of Chemical and Process Engineering, Rzeszów University of Technology, PL-35 959 Rzeszów, Poland.
Department of Chemical and Pharmaceutical Sciences, University of Ferrara, IT-44 121 Ferrara, Italy.
Visa övriga samt affilieringar
2015 (Engelska)Ingår i: Journal of Chromatography A, ISSN 0021-9673, E-ISSN 1873-3778, Vol. 1401, s. 52-59Artikel i tidskrift (Refereegranskat) Published
Abstract [en]

The importance of the generated temperature and pressure gradients in ultra-high-pressure liquid chromatography (UHPLC) are investigated and compared to high-pressure liquid chromatography (HPLC). The drug Omeprazole, together with three other model compounds (with different chemical characteristics, namely uncharged, positively and negatively charged) were used. Calculations of the complete temperature profile in the column at UHPLC conditions showed, in our experiments, a temperature difference between the inlet and outlet of 16 degrees C and a difference of 2 degrees C between the column center and the wall. Through van't Hoff plots, this information was used to single out the decrease in retention factor (k) solely due to the temperature gradient. The uncharged solute was least affected by temperature with a decrease in k of about 5% while for charged solutes the effect was more pronounced, with k decreases up to 14%. A pressure increase of 500 bar gave roughly 5% increase in k for the uncharged solute, while omeprazole and the other two charged solutes gave about 25, 20 and 15% increases in k, respectively. The stochastic model of chromatography was applied to estimate the dependence of the average number of adsorption/desorption events (n) and the average time spent by a molecule in the stationary phase (tau(s)) on temperature and pressure on peak shape for the tailing, basic solute. Increasing the temperature yielded an increase in n and decrease in tau(s) which resulted in less skew at high temperatures. With increasing pressure, the stochastic modeling gave interesting results for the basic solute showing that the skew of the peak increased with pressure. The conclusion is that pressure effects are more pronounced for both retention and peak shape than the temperature effects for the polar or charged compounds in our study. (C) 2015 Elsevier B.V. All rights reserved.

Ort, förlag, år, upplaga, sidor
Elsevier, 2015. Vol. 1401, s. 52-59
Nyckelord [en]
Liquid chromatography; Method transfer; UHPLC; Pressure; Temperature; Stochastic theory
Nationell ämneskategori
Polymerteknologi Organisk kemi Analytisk kemi
Forskningsämne
Kemiteknik
Identifikatorer
URN: urn:nbn:se:kau:diva-37297DOI: 10.1016/j.chroma.2015.05.002ISI: 000356550800007PubMedID: 26003622OAI: oai:DiVA.org:kau-37297DiVA, id: diva2:844553
Tillgänglig från: 2015-08-06 Skapad: 2015-08-06 Senast uppdaterad: 2017-12-06Bibliografiskt granskad
Ingår i avhandling
1. Fundamental and Regulatory Aspects of UHPLC in Pharmaceutical Analysis
Öppna denna publikation i ny flik eller fönster >>Fundamental and Regulatory Aspects of UHPLC in Pharmaceutical Analysis
2017 (Engelska)Doktorsavhandling, sammanläggning (Övrigt vetenskapligt)
Abstract [en]

Ultra-high performance liquid chromatography (UHPLC) provides a considerable increase in throughput compared to HPLC and a reduced solvent consumption. The implementation of UHPLC in pharmaceutical analysis, e.g. quality control, has accelerated in recent years and there is currently a mix of HPLC and UHPLC instrumentation within pharmaceutical companies. There are, however, technical and regulatory challenges converting a HPLC method to UHPLC making it difficult to take full advantage of UHPLC in regulatory-focused applications like quality control in pharmaceutical production.

Using chromatographic modelling and fundamental theory, this thesis investigated method conversion between HPLC and UHPLC. It reports on the influence of temperature gradients due to viscous heating, pressure effects and stationary phase properties on the separation performance. It also presents a regulatory concept for less regulatory interaction for minor changes to approved methods to support efficient life cycle management.

The higher pressure in UHPLC gave a retention increase of up to 40% as compared to conventional HPLC while viscous heating, instead, reduced retention and the net result was very solute dependent. Selectivity shifts were observed even between solutes with similar structure when switching between HPLC and UHPLC and an experimental method to predict such selectivity shifts was therefore developed. The peak shape was negatively affected by the increase in pressure for some solutes since secondary interactions between the solute and the stationary phase increased with pressure.

With the upcoming ICH Q12 guideline, it will be possible for the industry to convert existing methods to UHPLC in a more flexible way using the deeper understanding and the regulatory concept presented here as a case example.

Abstract [en]

Ultra-high performance liquid chromatography (UHPLC) provides a considerable increase in throughput compared to conventional HPLC and a reduced solvent consumption. The implementation of UHPLC in pharmaceutical analysis has accelerated in recent years and currently both instruments are used. There are, however, technical and regulatory challenges converting a HPLC method to UHPLC making it difficult to take full advantage of UHPLC in regulatory-focused applications like quality control in pharmaceutical production. In UHPLC, the column is packed with smaller particles than in HPLC resulting in higher pressure and viscous heating. Both the higher pressure and the higher temperature may cause changes in retention and selectivity making method conversion unpredictable.

Using chromatographic modelling and fundamental theory, this thesis investigates method conversion between HPLC and UHPLC. It reports on the influence of temperature gradients due to viscous heating, pressure effects and stationary phase properties on the separation performance. It also presents a regulatory concept for less regulatory interaction for minor changes to approved quality control methods and how predicable method conversion is achieved by improved understanding.

Ort, förlag, år, upplaga, sidor
Karlstad: Karlstads universitet, 2017. s. 75
Serie
Karlstad University Studies, ISSN 1403-8099 ; 2017:9
Nyckelord
Liquid chromatography, UHPLC, Pharmaceutical analysis, Adsorption isotherm, Design of experiments, Quality control
Nationell ämneskategori
Analytisk kemi
Forskningsämne
Kemi
Identifikatorer
urn:nbn:se:kau:diva-47852 (URN)978-91-7063-756-8 (ISBN)978-91-7063-757-5 (ISBN)
Disputation
2017-04-06, 9C204, Rejmersalen, Karlstads universitet, Universitetsgatan 2, Karlstad, 10:00 (Engelska)
Opponent
Handledare
Forskningsfinansiär
Vetenskapsrådet, 2015-04627ÅForsk (Ångpanneföreningens Forskningsstiftelse), 15/497
Tillgänglig från: 2017-03-08 Skapad: 2017-02-10 Senast uppdaterad: 2019-06-10Bibliografiskt granskad

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Förlagets fulltextPubMedhttp://www.sciencedirect.com/science/article/pii/S0021967315006585

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Åsberg, DennisSamuelsson, JörgenFornstedt, Torgny

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