Environmental chiral analysis of β-blockers: evaluation of different n-alkyl-modified SBA-15 mesoporous silicas as sorbents in solid-phase extraction

2018 ◽  
Vol 15 (6) ◽  
pp. 362 ◽  
Author(s):  
Mariana Silva ◽  
Sonia Morante-Zarcero ◽  
Damián Pérez-Quintanilla ◽  
María Luisa Marina ◽  
Isabel Sierra
Keyword(s):  
Electron Microscopy ◽  
Risk Assessment ◽  
Mesoporous Silica ◽  
Solid Phase Extraction ◽  
Water Samples ◽  
Solid Phase ◽  
Sewage Water ◽  
Chiral Analysis ◽  
Phase Extraction ◽  
Β Blockers

Environmental contextβ-Blockers are important chiral pharmaceuticals found as micropollutants in environmental waters as a result of incomplete removal during wastewater treatment. Because they display enantioselective toxicity, it is necessary to include chiral information in an environmental risk assessment. We have developed an analytical method using mesoporous silica for extracting β-blockers in water samples before their specific chiral analysis. AbstractThe extraction and preconcentration of chiral β-blockers in environmental water was evaluated by solid-phase extraction (SPE) employing an SBA-15 ordered mesoporous silica functionalised with alkyl chains of different length. The materials were characterised by X-ray diffraction, transmission electron microscopy, scanning electron microscopy, nitrogen adsorption–desorption isotherm measurements and elemental analysis. Important parameters influencing extraction efficiency, including the type and amount of sorbent and the breakthrough volume, were optimised. The results obtained showed that the organic chain length played an important role in the behaviour of these sorbents. Under optimised conditions, using 200 mg SBA-15-C8 as sorbent, a simple analytical method based on off-line SPE coupled to chiral capillary electrophoresis with diode array detection (SPE-chiral CE-DAD) was developed. Method detection and quantification limits were lower than 0.6 and 1.9 µg L −1 respectively for all enantiomers, with a preconcentration factor of 500-fold. The method was successfully applied to the chiral analysis of atenolol, metoprolol, pindolol and propranolol in river and sewage water samples. Satisfactory recoveries (between 86 ± 2 and 98 ± 1 %) and repeatability (relative standard deviation (RSD) < 9 %, n = 3) were obtained. Metoprolol was detected in sewage water at a concentration of 10.7 and 9.9 µg L−1 and an enantiomeric fraction of 0.52 and 0.48 for the first- and the second-migrating enantiomers respectively. These results emphasise the importance of enantioselective analysis for environmental risk assessment.

Mesoporous silica sorbent with gold nanoparticles for solid-phase extraction of organochlorine pesticides in water samples

2021 ◽  
pp. 462729
Author(s):  
Enric Pellicer-Castell ◽  
Carolina Belenguer-Sapiña ◽  
Pedro Amorós ◽  
Jamal El Haskouri ◽  
José Manuel Herrero-Martínez ◽  
...  
Keyword(s):  
Gold Nanoparticles ◽  
Mesoporous Silica ◽  
Solid Phase Extraction ◽  
Organochlorine Pesticides ◽  
Water Samples ◽  
Solid Phase ◽  
Phase Extraction ◽  
Pesticides In Water

Simultaneous extraction of permethrin diastereomers and deltamethrin in environmental water samples based on aperture regulated magnetic mesoporous silica

2020 ◽  
Vol 44 (37) ◽  
pp. 16152-16162
Author(s):  
Meixing Zhang ◽  
Jie Mei ◽  
Siying Lv ◽  
Jiahao Lai ◽  
Xiaoni Zheng ◽  
...  
Keyword(s):  
Mesoporous Silica ◽  
Solid Phase Extraction ◽  
Water Samples ◽  
Solid Phase ◽  
Magnetic Solid Phase Extraction ◽  
Environmental Water ◽  
Phase Extraction ◽  
Simultaneous Extraction ◽  
Magnetic Solid ◽  
Magnetic Mesoporous Silica

The aperture of KIT-6 can influence the recoveries of magnetic solid phase extraction.

Molecularly Imprinted Solid-Phase Extraction for Chlorpyrifos Determination in Water Samples

2010 ◽  
Vol 113-116 ◽  
pp. 947-951 ◽  
Author(s):  
Jun Liu ◽  
Ming Yang ◽  
Lu Feng Huai
Keyword(s):  
Solid Phase Extraction ◽  
Water Samples ◽  
Matrix Effects ◽  
Solid Phase ◽  
Final Analysis ◽  
Sewage Water ◽  
Phase Extraction ◽  
Simple Method ◽  
Molecularly Imprinted ◽  
The Matrix

The determination of chlorpyrifos at low ngL-1 levels in wastewater requires highly selective and sensitive analytical procedures. The removal of matrix components during sample preparation results in significant benefits towards reducing the matrix effects during GC analysis. Therefore this work describes a simple method to enrich and clean up chlorpyrifos from sewage water using molecularly imprinted solid phase extraction (MISPE). Final analysis was performed by gas chromatography. The performance of this method has been evaluated in water samples in terms of recovery, precision, and method quantification limit. Recovery for chlorpyrifos ranged between 99 and 105% with RSD values below 7.9%. The performance of the method was further emphasized by the study of different water samples. In these samples, chlorpyrifos were detected in concentration above method quantification limits ranging from 50 to 3000 ngL-1.

scholarly journals Magnetic Solid Phase Extraction using Magnetic Mesoporous Silica for Preconcentration of Organophosphorus Pesticides

2019 ◽  
Vol 8 (4) ◽  
pp. 6847-6852
Keyword(s):  
Mesoporous Silica ◽  
Solid Phase Extraction ◽  
Water Samples ◽  
High Performance ◽  
Solid Phase ◽  
Organophosphorus Pesticides ◽  
Magnetic Solid Phase Extraction ◽  
Phase Extraction ◽  
Magnetic Solid ◽  
Mcm 41

The present study describes the synthesis, characterization and application of two mesoporous silica material based coated magnetic nanoparticles namely Fe3O4 -SBA-15 and Fe3O4 -MCM-41 for the simultaneous preconcentration of three selected organophosphorus pesticides (OPPs) namely chlorpyrifos, diazinon and parathion methyl from water samples. The resultant sorbent material was physicochemically and morphologically characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and N2 adsorption analysis. OPPs pesticides extraction efficiency of two sorbents were evaluated through magnetic solid phase extraction (MSPE) using high performance liquid chromatography with ultraviolet detector (HPLC/UV). The main parameters affecting the sorbent efficiency namely extraction time and desorption solvent were optimized. Comparatively, Fe3O4 -SBA-15 achieved excellent percent recovery (97.5%) compared to the Fe3O4 -MCM-41 (87.1%) under optimum condition respectively. The result appealed that the Fe3O4 -SBA-15 composite was efficient sorbent with good capability for the preconcentration of selected OPPs from water samples.AThe present study describes the synthesis, characterization and application of two mesoporous silica material based coated magnetic nanoparticles namely Fe3O4 -SBA-15 and Fe3O4 -MCM-41 for the simultaneous preconcentration of three selected organophosphorus pesticides (OPPs) namely chlorpyrifos, diazinon and parathion methyl from water samples. The resultant sorbent material was physicochemically and morphologically characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and N2 adsorption analysis. OPPs pesticides extraction efficiency of two sorbents were evaluated through magnetic solid phase extraction (MSPE) using high performance liquid chromatography with ultraviolet detector (HPLC/UV). The main parameters affecting the sorbent efficiency namely extraction time and desorption solvent were optimized. Comparatively, Fe3O4 -SBA-15 achieved excellent percent recovery (97.5%) compared to the Fe3O4 -MCM-41 (87.1%) under optimum condition respectively. The result appealed that the Fe3O4 -SBA-15 composite was efficient sorbent with good capability for the preconcentration of selected OPPs from water samples.

Solid phase extraction of Pb(II) in water samples using a new hybrid inorganic-organic mesoporous silica prior to its determination by FAAS

2009 ◽  
Vol 165 (3-4) ◽  
pp. 291-298 ◽  
Author(s):  
Damián Pérez-Quintanilla ◽  
Alfredo Sánchez ◽  
Isabel del Hierro ◽  
Mariano Fajardo ◽  
Isabel Sierra
Keyword(s):  
Mesoporous Silica ◽  
Solid Phase Extraction ◽  
Water Samples ◽  
Solid Phase ◽  
Phase Extraction

scholarly journals Separation and determination of lead in human urine and water samples based on thiol functionalized mesoporous silica nanoparticles packed on cartridges by micro column fast micro solid-phase extraction

2019 ◽  
pp. 39-50 ◽  
Author(s):  
Maling Gou ◽  
*Baharak Bahrami Yarahmadi
Keyword(s):  
Mesoporous Silica ◽  
Solid Phase Extraction ◽  
Silica Nanoparticles ◽  
Water Samples ◽  
Solid Phase ◽  
Mesoporous Silica Nanoparticles ◽  
Electrothermal Atomic Absorption Spectrometry ◽  
Cellulose Membrane ◽  
Phase Extraction ◽  
Functionalized Mesoporous Silica

An efficient method based on thiol functionalized mesoporous silica nanoparticles (HS-MSNPs) was used for extraction of lead ions (PbII) from urine and water samples by packed column micro solid phase extraction (PC-MSPE). By procedure, 15 mg of HS-MSNPs packed in syringe cartridges (SC, 5 mL) with cellulose membrane and pH adjusting at 5.5-6.5.  Then, the lead of urine and water sample was efficiently extracted on HS-MSNPs after pushing the plunger of a syringe. Finally, the Pb (II) was back-extracted with inorganic acid solution and the remained solution determined by electrothermal atomic absorption spectrometry (ET-AAS). By optimization conditions, the enrichment factor, LOD, linear range and RSD% was obtained 24.8, 0.04 μg L-1, 0.12-5.5 μg L-1 and less than 5%, respectively for 5 mL of urine samples. The validation was confirmed by spiking of real samples and using certified reference material (CRM, NIST) in water and urine sample.

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