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Description
  • A fully automated HPLC column-switching method with fast sample pretreatment on a short micro-column was developed for sensitive and quantitative determination of non-steroidal anti-inflammatory drugs (ketoprofen, ibuprofen, sodium diclofenac and flurbiprofen) in human serum with UV detection. The serum samples were diluted 3 : 1, with 2% acetic acid in acetonitrile, and centrifuged at 4200g for 10 min. 200 mL of supernatant was injected directly into the HPLC system. An on-line sample clean-up was achieved on a pretreatment micro-column LiChrospher (R) RP-18 ADS 25 m-2.0 mm, 25 mm (Merck) with a washing mobile phase (acetonitrile : 0.085% phosphoric acid; 10 : 90) at a flow rate of 2.5 mu L min(-1). The valve switch to an analytical column was set at the 7th min in a back-flush mode. Separation of all antiflogistics and internal standard butylparaben was performed using a Chromolith Performance RP 18 100-4.6 mm column (Merck) and a mobile phase consisting of 0.085% phosphoric acid and acetonitrile in gradient mode. The column temperature was set at 45 degrees C and a flow rate of 1.0 mL min-1 and a UV detector at 210 nm. Standard and matrix calibrations were carried out under the optimal chromatographic conditions in the linearity range 7-2000 ng mL(-1) with good linearity correlation coefficients for all compounds are in the range 0.9956-0.9999, n }= 6. Limits of quantification were in the range 7-56 ng mL(-1). The accuracy of the method defined as a mean recovery was in the range 81.97-118.40%. Intra-day method precision was measured at three concentration levels and relative standard deviations were in the range 0.07-1.92%. The developed method showed high sample throughput, fully automated sample clean-up and analysis in time less than 17 min.
  • A fully automated HPLC column-switching method with fast sample pretreatment on a short micro-column was developed for sensitive and quantitative determination of non-steroidal anti-inflammatory drugs (ketoprofen, ibuprofen, sodium diclofenac and flurbiprofen) in human serum with UV detection. The serum samples were diluted 3 : 1, with 2% acetic acid in acetonitrile, and centrifuged at 4200g for 10 min. 200 mL of supernatant was injected directly into the HPLC system. An on-line sample clean-up was achieved on a pretreatment micro-column LiChrospher (R) RP-18 ADS 25 m-2.0 mm, 25 mm (Merck) with a washing mobile phase (acetonitrile : 0.085% phosphoric acid; 10 : 90) at a flow rate of 2.5 mu L min(-1). The valve switch to an analytical column was set at the 7th min in a back-flush mode. Separation of all antiflogistics and internal standard butylparaben was performed using a Chromolith Performance RP 18 100-4.6 mm column (Merck) and a mobile phase consisting of 0.085% phosphoric acid and acetonitrile in gradient mode. The column temperature was set at 45 degrees C and a flow rate of 1.0 mL min-1 and a UV detector at 210 nm. Standard and matrix calibrations were carried out under the optimal chromatographic conditions in the linearity range 7-2000 ng mL(-1) with good linearity correlation coefficients for all compounds are in the range 0.9956-0.9999, n }= 6. Limits of quantification were in the range 7-56 ng mL(-1). The accuracy of the method defined as a mean recovery was in the range 81.97-118.40%. Intra-day method precision was measured at three concentration levels and relative standard deviations were in the range 0.07-1.92%. The developed method showed high sample throughput, fully automated sample clean-up and analysis in time less than 17 min. (en)
Title
  • A fast on-line micro-column sample pretreatment with a HPLC column switching technique and large volume sample injection for determination of non-steroidal anti-inflammatory drugs in human serum
  • A fast on-line micro-column sample pretreatment with a HPLC column switching technique and large volume sample injection for determination of non-steroidal anti-inflammatory drugs in human serum (en)
skos:prefLabel
  • A fast on-line micro-column sample pretreatment with a HPLC column switching technique and large volume sample injection for determination of non-steroidal anti-inflammatory drugs in human serum
  • A fast on-line micro-column sample pretreatment with a HPLC column switching technique and large volume sample injection for determination of non-steroidal anti-inflammatory drugs in human serum (en)
skos:notation
  • RIV/00216208:11160/13:10146042!RIV14-MSM-11160___
http://linked.open...avai/predkladatel
http://linked.open...avai/riv/aktivita
http://linked.open...avai/riv/aktivity
  • I, S
http://linked.open...iv/cisloPeriodika
  • 21
http://linked.open...vai/riv/dodaniDat
http://linked.open...aciTvurceVysledku
http://linked.open.../riv/druhVysledku
http://linked.open...iv/duvernostUdaju
http://linked.open...titaPredkladatele
http://linked.open...dnocenehoVysledku
  • 58607
http://linked.open...ai/riv/idVysledku
  • RIV/00216208:11160/13:10146042
http://linked.open...riv/jazykVysledku
http://linked.open.../riv/klicovaSlova
  • LC-MS; UV detection; horse plasma; mass spectrometry; pharmaceutical formulations; human plasma; restricted access materials; solid phase extraction; high performance liquid chromatography (en)
http://linked.open.../riv/klicoveSlovo
http://linked.open...odStatuVydavatele
  • US - Spojené státy americké
http://linked.open...ontrolniKodProRIV
  • [EB43D81FC5D8]
http://linked.open...i/riv/nazevZdroje
  • Analytical Methods
http://linked.open...in/vavai/riv/obor
http://linked.open...ichTvurcuVysledku
http://linked.open...cetTvurcuVysledku
http://linked.open...UplatneniVysledku
http://linked.open...v/svazekPeriodika
  • 5
http://linked.open...iv/tvurceVysledku
  • Solich, Petr
  • Šatínský, Dalibor
  • Brabcová, Ivana
http://linked.open...ain/vavai/riv/wos
  • 000325722600044
issn
  • 1759-9660
number of pages
http://bibframe.org/vocab/doi
  • 10.1039/c3ay40505b
http://localhost/t...ganizacniJednotka
  • 11160
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