改进的QuEChERS结合超高效液相色谱-串联质谱法快速测定地表水中双酚类物质
Chromatography combined with mass spectrometry is the most commonly used detection technology, and it offers the advantages of high sensitivity and high selectivity. However, the contents of bisphenols (BPs) in water samples are at the ng/L level. Even if the BPs contents are determined by mass spec...
Autores principales: | , , , , , , |
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Formato: | Online Artículo Texto |
Lenguaje: | English |
Publicado: |
Editorial board of Chinese Journal of Chromatography
2022
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Materias: | |
Acceso en línea: | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9404128/ https://www.ncbi.nlm.nih.gov/pubmed/34985216 http://dx.doi.org/10.3724/SP.J.1123.2021.03010 |
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author | TAN, Xuerong ZHAO, Bin LU, Jianwei LIU, Shaoying GOU, Weini YANG, Rong ZUO, Peng |
author_facet | TAN, Xuerong ZHAO, Bin LU, Jianwei LIU, Shaoying GOU, Weini YANG, Rong ZUO, Peng |
author_sort | TAN, Xuerong |
collection | PubMed |
description | Chromatography combined with mass spectrometry is the most commonly used detection technology, and it offers the advantages of high sensitivity and high selectivity. However, the contents of bisphenols (BPs) in water samples are at the ng/L level. Even if the BPs contents are determined by mass spectrometry, the samples must be pretreated and enriched. A quick, easy, inexpensive, effective, rugged, and safe technique (QuEChERS) can offer advantages such as cost effectiveness and time efficiency. The application of QuEChERS is currently extended to the analysis of contaminants in food and water samples. In this work, QuEChERS coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was proposed for the determination of eight BPs in surface water. Method optimization was carried out in terms of process efficiency (PE), which included the matrix effect (ME) and extraction recovery (RE). First, the water samples were extracted with 10 mL ethyl acetate and cleaned with 50 mg primary secondary amine (PSA) and 50 mg graphitized carbon black (GCB). Then, the organic layer was collected and evaporated to dryness under nitrogen flow (40 ℃). Finally, the extracts were redissolved in 0.5 mL of a methanol-water (1:1, v/v) mixture and subjected to UPLC-MS/MS analysis. Chromatographic separation was accomplished on a Waters ACQUITY UPLC BEH C(18) column (100 mm×2.1 mm, 1.7 μm) with gradient elution. Methanol and 0.1 mmol/L ammonium bicarbonate aqueous solution were used as the mobile phases. The eight BPs were analyzed by MS/MS with negative electrospray ionization (ESI(-)) and in the multiple reaction monitoring (MRM) mode. The matrix matching external standard method was used for quantitative determination. The eight compounds could be analyzed within 8 min. Under the optimized conditions, the calibration curves showed good linearities for the eight BPs, and the coefficients of determination (R(2)) were greater than 0.9990. The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) were in the ranges of 0.1-2.3 ng/L and 0.3-6.1 ng/L, respectively. The average recoveries of the eight BPs in river water samples were 78.8%-116.6%, and the corresponding relative standard deviations (RSDs) were 1.8%-9.0% (n=6). This method was applied to the analysis of BPs pollution in Guangyuan section of Jialing river and its tributaries, and widespread pollution was confirmed. The detection rate of BPA was 100% with a content of 6.15-90.03 ng/L, and the detection rate of BPS was 91%, with the contents being in the range not detected (nd) to 4.63 ng/L. The method established in this study allowed for the rapid enrichment and purification of the eight BPs in water. With its advantages of simplicity, rapidness, high sensitivity, and low cost, the method can be used for the rapid determination of trace BPs in surface water such as lake water and river water. |
format | Online Article Text |
id | pubmed-9404128 |
institution | National Center for Biotechnology Information |
language | English |
publishDate | 2022 |
publisher | Editorial board of Chinese Journal of Chromatography |
record_format | MEDLINE/PubMed |
spelling | pubmed-94041282022-09-14 改进的QuEChERS结合超高效液相色谱-串联质谱法快速测定地表水中双酚类物质 TAN, Xuerong ZHAO, Bin LU, Jianwei LIU, Shaoying GOU, Weini YANG, Rong ZUO, Peng Se Pu Articles Chromatography combined with mass spectrometry is the most commonly used detection technology, and it offers the advantages of high sensitivity and high selectivity. However, the contents of bisphenols (BPs) in water samples are at the ng/L level. Even if the BPs contents are determined by mass spectrometry, the samples must be pretreated and enriched. A quick, easy, inexpensive, effective, rugged, and safe technique (QuEChERS) can offer advantages such as cost effectiveness and time efficiency. The application of QuEChERS is currently extended to the analysis of contaminants in food and water samples. In this work, QuEChERS coupled with ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was proposed for the determination of eight BPs in surface water. Method optimization was carried out in terms of process efficiency (PE), which included the matrix effect (ME) and extraction recovery (RE). First, the water samples were extracted with 10 mL ethyl acetate and cleaned with 50 mg primary secondary amine (PSA) and 50 mg graphitized carbon black (GCB). Then, the organic layer was collected and evaporated to dryness under nitrogen flow (40 ℃). Finally, the extracts were redissolved in 0.5 mL of a methanol-water (1:1, v/v) mixture and subjected to UPLC-MS/MS analysis. Chromatographic separation was accomplished on a Waters ACQUITY UPLC BEH C(18) column (100 mm×2.1 mm, 1.7 μm) with gradient elution. Methanol and 0.1 mmol/L ammonium bicarbonate aqueous solution were used as the mobile phases. The eight BPs were analyzed by MS/MS with negative electrospray ionization (ESI(-)) and in the multiple reaction monitoring (MRM) mode. The matrix matching external standard method was used for quantitative determination. The eight compounds could be analyzed within 8 min. Under the optimized conditions, the calibration curves showed good linearities for the eight BPs, and the coefficients of determination (R(2)) were greater than 0.9990. The limits of detection (LODs, S/N=3) and limits of quantification (LOQs, S/N=10) were in the ranges of 0.1-2.3 ng/L and 0.3-6.1 ng/L, respectively. The average recoveries of the eight BPs in river water samples were 78.8%-116.6%, and the corresponding relative standard deviations (RSDs) were 1.8%-9.0% (n=6). This method was applied to the analysis of BPs pollution in Guangyuan section of Jialing river and its tributaries, and widespread pollution was confirmed. The detection rate of BPA was 100% with a content of 6.15-90.03 ng/L, and the detection rate of BPS was 91%, with the contents being in the range not detected (nd) to 4.63 ng/L. The method established in this study allowed for the rapid enrichment and purification of the eight BPs in water. With its advantages of simplicity, rapidness, high sensitivity, and low cost, the method can be used for the rapid determination of trace BPs in surface water such as lake water and river water. Editorial board of Chinese Journal of Chromatography 2022-01-08 /pmc/articles/PMC9404128/ /pubmed/34985216 http://dx.doi.org/10.3724/SP.J.1123.2021.03010 Text en https://creativecommons.org/licenses/by/4.0/本文是开放获取文章,遵循CC BY 4.0协议 https://creativecommons.org/licenses/by/4.0/This is an open access article distributed under the terms of the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original author and source are credited. |
spellingShingle | Articles TAN, Xuerong ZHAO, Bin LU, Jianwei LIU, Shaoying GOU, Weini YANG, Rong ZUO, Peng 改进的QuEChERS结合超高效液相色谱-串联质谱法快速测定地表水中双酚类物质 |
title | 改进的QuEChERS结合超高效液相色谱-串联质谱法快速测定地表水中双酚类物质 |
title_full | 改进的QuEChERS结合超高效液相色谱-串联质谱法快速测定地表水中双酚类物质 |
title_fullStr | 改进的QuEChERS结合超高效液相色谱-串联质谱法快速测定地表水中双酚类物质 |
title_full_unstemmed | 改进的QuEChERS结合超高效液相色谱-串联质谱法快速测定地表水中双酚类物质 |
title_short | 改进的QuEChERS结合超高效液相色谱-串联质谱法快速测定地表水中双酚类物质 |
title_sort | 改进的quechers结合超高效液相色谱-串联质谱法快速测定地表水中双酚类物质 |
topic | Articles |
url | https://www.ncbi.nlm.nih.gov/pmc/articles/PMC9404128/ https://www.ncbi.nlm.nih.gov/pubmed/34985216 http://dx.doi.org/10.3724/SP.J.1123.2021.03010 |
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