Normal phase HPLC/FT-IR detection and identification of β-cypermethrins by the flow-through cell method

Advantages and limitations

Krisztina István, G. Keresztury, J. Fekete

Research output: Contribution to journalArticle

6 Citations (Scopus)

Abstract

The capabilities and limitations of on-line FT-IR spectroscopic detection during normal phase HPLC separation have been examined and evaluated as applied to a practical analytical problem, using a commercial IR micro flow-through cell as an interface in conjunction with an up-to-date high speed, high sensitivity FT-IR spectrometer, and dedicated data processing utilities. It has been shown that the usual chromatographic mobile phases containing polar modifiers can be used in such measurements, although the technique has definite limitations depending on the spectroscopic properties of the mobile phases and the analytes in question. In case of analytes having strong IR features in regions clear from mobile phase absorption, IR chromatograms are suitable for major component detection, whereas narrow-region chemigram-type detection tuned to selected absorption bands of the target compound is more successful than Gram-Schmidt reconstructed chromatograms generated from full-range IR spectra. Quantitative determination of the two major diastereomers in the β-cypermethrin sample using the "carbonyl chemigram" has shown good linearity in the concentration range from 0.3 to 4.0 mg/mL. The value of 1.0 mg/mL proved to be the identification limit still allowing spectral discrimination of diastereomers, while the detection limit for the β-cypermethrins examined was 0.3 mg/mL in most mobile phases, but was estimated to be 0.1 mg/mL in acetonitrile/n-hexane (AN/nHEX).

Original languageEnglish
Pages (from-to)407-421
Number of pages15
JournalJournal of Liquid Chromatography and Related Technologies
Volume28
Issue number3
DOIs
Publication statusPublished - 2005

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High Pressure Liquid Chromatography
Infrared spectrometers
Phase separation
Limit of Detection
Absorption spectra
cypermethrin
n-hexane
acetonitrile

Keywords

  • Cypermethrin
  • Flow-through cell method
  • HPLC/FT-IR
  • Infrared chemigram
  • Normal phase chromatography

ASJC Scopus subject areas

  • Analytical Chemistry
  • Clinical Biochemistry

Cite this

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title = "Normal phase HPLC/FT-IR detection and identification of β-cypermethrins by the flow-through cell method: Advantages and limitations",
abstract = "The capabilities and limitations of on-line FT-IR spectroscopic detection during normal phase HPLC separation have been examined and evaluated as applied to a practical analytical problem, using a commercial IR micro flow-through cell as an interface in conjunction with an up-to-date high speed, high sensitivity FT-IR spectrometer, and dedicated data processing utilities. It has been shown that the usual chromatographic mobile phases containing polar modifiers can be used in such measurements, although the technique has definite limitations depending on the spectroscopic properties of the mobile phases and the analytes in question. In case of analytes having strong IR features in regions clear from mobile phase absorption, IR chromatograms are suitable for major component detection, whereas narrow-region chemigram-type detection tuned to selected absorption bands of the target compound is more successful than Gram-Schmidt reconstructed chromatograms generated from full-range IR spectra. Quantitative determination of the two major diastereomers in the β-cypermethrin sample using the {"}carbonyl chemigram{"} has shown good linearity in the concentration range from 0.3 to 4.0 mg/mL. The value of 1.0 mg/mL proved to be the identification limit still allowing spectral discrimination of diastereomers, while the detection limit for the β-cypermethrins examined was 0.3 mg/mL in most mobile phases, but was estimated to be 0.1 mg/mL in acetonitrile/n-hexane (AN/nHEX).",
keywords = "Cypermethrin, Flow-through cell method, HPLC/FT-IR, Infrared chemigram, Normal phase chromatography",
author = "Krisztina Istv{\'a}n and G. Keresztury and J. Fekete",
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AU - István, Krisztina

AU - Keresztury, G.

AU - Fekete, J.

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N2 - The capabilities and limitations of on-line FT-IR spectroscopic detection during normal phase HPLC separation have been examined and evaluated as applied to a practical analytical problem, using a commercial IR micro flow-through cell as an interface in conjunction with an up-to-date high speed, high sensitivity FT-IR spectrometer, and dedicated data processing utilities. It has been shown that the usual chromatographic mobile phases containing polar modifiers can be used in such measurements, although the technique has definite limitations depending on the spectroscopic properties of the mobile phases and the analytes in question. In case of analytes having strong IR features in regions clear from mobile phase absorption, IR chromatograms are suitable for major component detection, whereas narrow-region chemigram-type detection tuned to selected absorption bands of the target compound is more successful than Gram-Schmidt reconstructed chromatograms generated from full-range IR spectra. Quantitative determination of the two major diastereomers in the β-cypermethrin sample using the "carbonyl chemigram" has shown good linearity in the concentration range from 0.3 to 4.0 mg/mL. The value of 1.0 mg/mL proved to be the identification limit still allowing spectral discrimination of diastereomers, while the detection limit for the β-cypermethrins examined was 0.3 mg/mL in most mobile phases, but was estimated to be 0.1 mg/mL in acetonitrile/n-hexane (AN/nHEX).

AB - The capabilities and limitations of on-line FT-IR spectroscopic detection during normal phase HPLC separation have been examined and evaluated as applied to a practical analytical problem, using a commercial IR micro flow-through cell as an interface in conjunction with an up-to-date high speed, high sensitivity FT-IR spectrometer, and dedicated data processing utilities. It has been shown that the usual chromatographic mobile phases containing polar modifiers can be used in such measurements, although the technique has definite limitations depending on the spectroscopic properties of the mobile phases and the analytes in question. In case of analytes having strong IR features in regions clear from mobile phase absorption, IR chromatograms are suitable for major component detection, whereas narrow-region chemigram-type detection tuned to selected absorption bands of the target compound is more successful than Gram-Schmidt reconstructed chromatograms generated from full-range IR spectra. Quantitative determination of the two major diastereomers in the β-cypermethrin sample using the "carbonyl chemigram" has shown good linearity in the concentration range from 0.3 to 4.0 mg/mL. The value of 1.0 mg/mL proved to be the identification limit still allowing spectral discrimination of diastereomers, while the detection limit for the β-cypermethrins examined was 0.3 mg/mL in most mobile phases, but was estimated to be 0.1 mg/mL in acetonitrile/n-hexane (AN/nHEX).

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