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Dual gradient LC method for the determination of pharmaceutical residues in environmental samples using a monolithic silica reversed phase column

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posted on 2023-05-16, 20:05 authored by Bones, J, Nesterenko, PN, Thomas, K, Brett PaullBrett Paull
Detailed below is a simple reversed-phase liquid chromatography (RP-LC) method for the simultaneous separation of up to 21 acidic, basic, and neutral pharmaceuticals using Merck Chromolith Performance RP-C18e monolithic columns with direct ultraviolet (UV) absorption detection. By simultaneously applying a solvent elution gradient program with a mobile phase flow gradient, both a decrease in the overall analysis time and a general increase in peak efficiencies were observed. Mobile phase pH and buffer concentration were optimised using the overall resolution product under applied gradient conditions. Under optimised conditions peak area reproducibility (n = 6) ranged between 0.4 and 9.3%, determined at the method LOQ level. For real sample analysis pharmaceutical residues were extracted using an optimised solid phase extraction (SPE) procedure, utilising Strata-X extraction cartridges, which overall provided the highest relative recovery data in comparison with four other commercially available SPE sorbents (17 out of 20 residues investigated had recoveries over 70%). Complete method precision, including all sample pre-treatment and LC analysis for six spiked river water samples at the 1 and 2 μgL-1 level was between 10 and 29%. Using 1L volumes of 1 μgL-1 spiked estuarine water samples, the majority of detection limits were found to be in the 10-50 ng L-1 range. © 2006 Taylor & Francis.

History

Publication title

International Journal of Environmental Analytical Chemistry

Volume

86

Issue

7

Pagination

487-504

ISSN

0306-7319

Department/School

School of Natural Sciences

Publisher

Taylor & Francis Ltd.

Place of publication

United Kingdom

Repository Status

  • Restricted

Socio-economic Objectives

Expanding knowledge in the chemical sciences

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