Mixed Matrix Membrane Tip Extraction Coupled with UPLC–MS/MS for the Monitoring of Nonsteroidal Anti-Inflammatory Drugs in Water Samples

An ultra-performance liquid chromatography−tandem mass spectrometry (UPLC−MS/MS) method, in combination with a mixed matrix membrane microextraction method for the quantification of nonsteroidal anti-inflammatory drugs (NSAIDs) in environmental water samples, is reported. The ext...

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Main Authors: Thipashini Ganesan, Nurul Hazirah Mukhtar, Hong Ngee Lim, Hong Heng See
Format: Article
Language:English
Published: MDPI AG 2020-03-01
Series:Separations
Subjects:
Online Access:https://www.mdpi.com/2297-8739/7/1/19
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author Thipashini Ganesan
Nurul Hazirah Mukhtar
Hong Ngee Lim
Hong Heng See
author_facet Thipashini Ganesan
Nurul Hazirah Mukhtar
Hong Ngee Lim
Hong Heng See
author_sort Thipashini Ganesan
collection DOAJ
description An ultra-performance liquid chromatography&#8722;tandem mass spectrometry (UPLC&#8722;MS/MS) method, in combination with a mixed matrix membrane microextraction method for the quantification of nonsteroidal anti-inflammatory drugs (NSAIDs) in environmental water samples, is reported. The extraction device was prepared by casting well-dispersed polymeric bonded octadecyl (C<sub>18</sub>) particles in a cellulose triacetate matrix solution onto commercially available 200 &#956;L micropipette tips. The membrane formed contains 25% of the adsorbent loading amount and was firmly attached to the inner wall of the membrane tip. The dynamic extraction was performed by withdrawing and dispensing the sample solution through the tip device for effective analyte adsorption, followed by the analyte desorption process into 40 &#956;L of methanol and acetonitrile (1:1) prior to UPLC&#8722;MS/MS analysis. NSAIDs&#8212;namely diclofenac, ibuprofen, indoprofen, naproxen and sulindac&#8212;were chosen as targeted analytes. Several extraction parameters were comprehensively optimized, including sample pH value, ionic strength, dynamic extraction cycle, desorption solvent and desorption time. The optimized conditions demonstrated a linear range from 0.25 to 500 ng L<sup>&#8722;1</sup>, with correlation coefficients (<i>r</i><sup>2</sup>) from 0.9988 to 0.9992 and detection limits ranging from 0.08 to 0.40 ng L<sup>&#8722;1</sup>. The recoveries of the spiked water samples were between 92% and 99% and exhibited excellent precision relative to standard deviations (RSDs &#8804; 4.9%), and enrichment factors (EFs) were at 201&#8722;249 for the developed approach.
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spelling doaj.art-b9303ba1aa4b467886b1236fcea58a4a2022-12-22T02:57:57ZengMDPI AGSeparations2297-87392020-03-01711910.3390/separations7010019separations7010019Mixed Matrix Membrane Tip Extraction Coupled with UPLC–MS/MS for the Monitoring of Nonsteroidal Anti-Inflammatory Drugs in Water SamplesThipashini Ganesan0Nurul Hazirah Mukhtar1Hong Ngee Lim2Hong Heng See3Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia Centre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia Department of Chemistry, Faculty of Science, Universiti Putra Malaysia, 43400 Serdang, Selangor, MalaysiaCentre for Sustainable Nanomaterials, Ibnu Sina Institute for Scientific and Industrial Research, Universiti Teknologi Malaysia, 81310 UTM Johor Bahru, Johor, Malaysia An ultra-performance liquid chromatography&#8722;tandem mass spectrometry (UPLC&#8722;MS/MS) method, in combination with a mixed matrix membrane microextraction method for the quantification of nonsteroidal anti-inflammatory drugs (NSAIDs) in environmental water samples, is reported. The extraction device was prepared by casting well-dispersed polymeric bonded octadecyl (C<sub>18</sub>) particles in a cellulose triacetate matrix solution onto commercially available 200 &#956;L micropipette tips. The membrane formed contains 25% of the adsorbent loading amount and was firmly attached to the inner wall of the membrane tip. The dynamic extraction was performed by withdrawing and dispensing the sample solution through the tip device for effective analyte adsorption, followed by the analyte desorption process into 40 &#956;L of methanol and acetonitrile (1:1) prior to UPLC&#8722;MS/MS analysis. NSAIDs&#8212;namely diclofenac, ibuprofen, indoprofen, naproxen and sulindac&#8212;were chosen as targeted analytes. Several extraction parameters were comprehensively optimized, including sample pH value, ionic strength, dynamic extraction cycle, desorption solvent and desorption time. The optimized conditions demonstrated a linear range from 0.25 to 500 ng L<sup>&#8722;1</sup>, with correlation coefficients (<i>r</i><sup>2</sup>) from 0.9988 to 0.9992 and detection limits ranging from 0.08 to 0.40 ng L<sup>&#8722;1</sup>. The recoveries of the spiked water samples were between 92% and 99% and exhibited excellent precision relative to standard deviations (RSDs &#8804; 4.9%), and enrichment factors (EFs) were at 201&#8722;249 for the developed approach.https://www.mdpi.com/2297-8739/7/1/19microextractionmixed matrix membranesample preparationnsaidsuplc–ms/ms
spellingShingle Thipashini Ganesan
Nurul Hazirah Mukhtar
Hong Ngee Lim
Hong Heng See
Mixed Matrix Membrane Tip Extraction Coupled with UPLC–MS/MS for the Monitoring of Nonsteroidal Anti-Inflammatory Drugs in Water Samples
Separations
microextraction
mixed matrix membrane
sample preparation
nsaids
uplc–ms/ms
title Mixed Matrix Membrane Tip Extraction Coupled with UPLC–MS/MS for the Monitoring of Nonsteroidal Anti-Inflammatory Drugs in Water Samples
title_full Mixed Matrix Membrane Tip Extraction Coupled with UPLC–MS/MS for the Monitoring of Nonsteroidal Anti-Inflammatory Drugs in Water Samples
title_fullStr Mixed Matrix Membrane Tip Extraction Coupled with UPLC–MS/MS for the Monitoring of Nonsteroidal Anti-Inflammatory Drugs in Water Samples
title_full_unstemmed Mixed Matrix Membrane Tip Extraction Coupled with UPLC–MS/MS for the Monitoring of Nonsteroidal Anti-Inflammatory Drugs in Water Samples
title_short Mixed Matrix Membrane Tip Extraction Coupled with UPLC–MS/MS for the Monitoring of Nonsteroidal Anti-Inflammatory Drugs in Water Samples
title_sort mixed matrix membrane tip extraction coupled with uplc ms ms for the monitoring of nonsteroidal anti inflammatory drugs in water samples
topic microextraction
mixed matrix membrane
sample preparation
nsaids
uplc–ms/ms
url https://www.mdpi.com/2297-8739/7/1/19
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AT hongngeelim mixedmatrixmembranetipextractioncoupledwithuplcmsmsforthemonitoringofnonsteroidalantiinflammatorydrugsinwatersamples
AT honghengsee mixedmatrixmembranetipextractioncoupledwithuplcmsmsforthemonitoringofnonsteroidalantiinflammatorydrugsinwatersamples