scholarly journals Polycarbonate Microchip Containing CuBTC-Monopol Monolith for Solid-Phase Extraction of Dyes

2020 ◽  
Vol 2020 ◽  
pp. 1-15 ◽  
Author(s):  
Eman Alzahrani
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Solvent System ◽  
Butyl Methacrylate ◽  
Phase Extraction ◽  
Ethanolic Solution ◽  
Toxic Dyes ◽  
Relative Standard ◽  
Uv Lamp ◽  
Dye Extraction

In the present study, preparation of CuBTC-monopol monoliths for use within the microchip solid phase extraction was undertaken through a 20-min UV lamp-assisted polymerization for 2,2-dimethoxy-2-phenyl acetophenone (DMPA), butyl methacrylate (BMA), and ethylene dimethacrylate (EDMA) alongside inclusion of the porogenic solvent system (1-propanol and methanol (1 : 1)). The resultant coating underwent coating using CuBTC nanocrystals in ethanolic solution of ethanolic solution of 1,3,5-benzenetricarboxylic acid (H3BTC, 10 mM) and 10 mM copper(II) acetate Cu(CH3COO)2. This paper reports enhanced extraction, characterization, and synthesis studies for porous CuBTC metal organic frameworks that are marked by different methods including SEM/EDAX analysis, atomic force microscopy (AFM), and Fourier-transform infrared spectroscopy (FT-IR). The evaluation of the microchip’s performance was undertaken as sorbent through retrieval of six toxic dyes (anionic and cationic dyes). Various parameters (desorption and extraction step flow rates, volume of desorption solvent, volume of sample, and type of desorption solvent) were examined to optimize dye extraction using fabricated microchips. The result indicated that CuBTC-monopol monoliths were permeable with the ability of removing impurities and attained high toxic dye extraction recovery (83.4–99.9%). The assessment of reproducibility for chip-to-chip was undertaken by computing the relative standard deviations (RSDs) of the six dyes in extraction. The interbatch and intrabatch RSDs ranged between 3.8 and 6.9% and 2.3 and 4.8%. Such features showed that fabricated CuBTC-monopol monolithic disk polycarbonate microchips have the potential of extracting toxic dyes that could be utilized for treating wastewater.

Factorial Design Optimisation of Solid Phase Extraction for Preconcentration of Parabens in Wastewater Using Ultra-High Performance Liquid Chromatography Triple Quadrupole Mass Spectrometry

2020 ◽  
Vol 16 (4) ◽  
pp. 436-446
Author(s):  
Vallerie A. Muckoya ◽  
Philiswa N. Nomngongo ◽  
Jane C. Ngila
Keyword(s):  
Solid Phase Extraction ◽  
Formic Acid ◽  
Factorial Design ◽  
Solid Phase ◽  
Treatment Plant ◽  
Phase Extraction ◽  
Limit Of Quantification ◽  
Analytical Technique ◽  
Relative Standard ◽  
Simulated Wastewater

Background: Parabens are synthetic esters used extensively as preservatives and/or bactericides in personal care personal products. Objective: Development and validation of a novel robust chemometric assisted analytical technique with superior analytical performances for the determination of ethylparaben, methylparaben and propylparaben, using simulated wastewater matrix. Methods: An automated Solid Phase Extraction (SPE) method coupled with liquid chromatographymass spectrometry was applied in this study. A gradient elution programme comprising of 0.1% formic acid in deionised water (A) and 0.1% formic acid in Methanol (B) was employed on a 100 x 2.1 mm, 3.0 μm a particle size biphenyl column. Two-level (2k) full factorial design coupled with response surface methodology was used for optimisation and investigation of SPE experimental variables that had the most significant outcome of the analytical response. Results: According to the analysis of variance (ANOVA), sample pH and eluent volume were statistically the most significant parameters. The method developed was validated for accuracy, precision, Limits of Detection (LOD) and Limit of Quantification (LOQ) and linearity. The LOD and LOQ established under those optimised conditions varied between 0.04-0.12 μgL−1 and 0.14-0.40 μgL−1 respectively. The use of matrix-matched external calibration provided extraction recoveries between 78-128% with relative standard deviations at 2-11% for two spike levels (10 and 100 μgL-1) in three different water matrices (simulated wastewater, influent and effluent water). Conclusion: The newly developed method was applied successfully to the analyses of parabens in wastewater samples at different sampling points of a wastewater treatment plant, revealing concentrations of up to 3 μgL−1.

Green Dispersive Micro Solid-Phase Extraction using Multiwalled Carbon Nanotubes for Preconcentration and Determination of Cadmium and Lead in Food, Water, and Tobacco Samples

2020 ◽  
Vol 16 (4) ◽  
pp. 381-392
Author(s):  
Ayman A. Gouda ◽  
Ali H. Amin ◽  
Ibrahim S. Ali ◽  
Zakia Al Malah
Keyword(s):  
Carbon Nanotubes ◽  
Solid Phase Extraction ◽  
Multiwalled Carbon Nanotubes ◽  
Solid Phase ◽  
Certified Reference Materials ◽  
Phase Extraction ◽  
Multiwalled Carbon ◽  
Flame Atomic Absorption ◽  
Relative Standard ◽  
Separation And Preconcentration

Background: Cadmium (Cd2+) and lead (Pb2+) have acute and chronic effects on humans and other living organisms. In the present work, new, green and accurate dispersive micro solid-phase extraction (DμSPE) method for the separation and preconcentration of trace amounts of cadmium (Cd2+) and lead (Pb2+) ions in various food, water and tobacco samples collected from Saudi Arabia prior to its Flame Atomic Absorption Spectrometric (FAAS) determinations was developed. Methods: The proposed method was based on a combination of oxidized multiwalled carbon nanotubes (O-MWCNTs) with a new chelating agent 5-benzyl-4-[4-methoxybenzylideneamino)-4H- 1,2,4-triazole-3-thiol (BMBATT) to enrich and separate trace levels of Cd2+ and Pb2+. The effect of separation parameters was investigated. The validation of the proposed preconcentration procedure was performed using certified reference materials. Results: Analyte recovery values ranged from 95-102%, indicating that the method is highly accurate. Furthermore, precision was demonstrated by the relative standard deviation (RSD < 3.0%). The limits of detection were 0.08 and 0.1 μg L−1 for Cd2+ and Pb2+ ions, respectively. The preconcentration factor was 200. Conclusion: The proposed method was used for the estimation of Cd2+ and Pb2+ ion content in various real samples, and satisfactory results were obtained. The proposed method has high adsorption capacity, rapid adsorption equilibrium, extremely low LODs, high preconcentration factors and shortens the time of sample preparation in comparison to classical SPE.

Development of a solid-phase extraction – spectrofluorimetric method for trace glutathione determination

2011 ◽  
Vol 89 (4) ◽  
pp. 517-523 ◽  
Author(s):  
Ke-Jing Huang ◽  
Cong-Hui Han ◽  
Ying-Ying Wu ◽  
Chao-Qun Han ◽  
De-Jun Niu ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Calibration Graph ◽  
Extraction Column ◽  
Phase Extraction ◽  
Selective Reaction ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A simple and efficient solid-phase extraction – spectrofluorimetric method has been developed to determine glutathione (GSH). Fluorescent probe N-(4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacene-3-yl)methyl)iodoacetamide (BODIPY Fl-C1-IA) was used as the derivatization reagent. The procedure was based on a BODIPY Fl-C1-IA selective reaction with GSH to form the highly fluorescent product BODIPY Fl-C1-IA–GSH, using a solid-phase extraction column and spectrofluorimetric determination. The variables affecting analytical performance were studied and optimized. The calibration graph using the preconcentration system for GSH was linear over the range of 1–200 nmol/L with a limit of detection of 0.05 nmol/L (signal-to-noise ratio = 3). The relative standard deviation for six replicate determinations of GSH at the 100 nmol/L concentration level was 3.9%. The method was applied to water samples and average recoveries between 87.5% and 111.5% were obtained for spiked samples.

scholarly journals Solid-Phase Extraction and Reverse-Phase HPLC: Application to Study the Urinary Excretion Pattern of Benzophenone-3 and its Metabolite 2,4-Dihydroxybenzophenone in Human Urine

2008 ◽  
Vol 3 ◽  
pp. ACI.S396 ◽  
Author(s):  
Helena Gonzalez ◽  
Carl-Eric Jacobson ◽  
Ann-Marie Wennberg ◽  
Olle Larkö ◽  
Anne Farbrot
Keyword(s):  
Solid Phase Extraction ◽  
Urinary Excretion ◽  
Human Urine ◽  
Solid Phase ◽  
Whole Body ◽  
Phase Extraction ◽  
Reverse Phase Hplc ◽  
Reverse Phase ◽  
Excretion Pattern ◽  
Relative Standard

Background Benzophenone-3 (BZ-3) is a common ultraviolet (UV) absorbing compound in sunscreens. It is the most bioavailable species of all UV-absorbing compounds after topical application and can be found in plasma and urine. Objectives The aim of this study was to develop a reverse-phase high performance liquid chromatography (HPLC) method for determining the amounts BZ-3 and its metabolite 2,4-dihydroxybenzophenone (DHB) in human urine. The method had to be suitable for handling a large number of samples. It also had to be rapid and simple, but still sensitive, accurate and reproducible. The assay was applied to study the urinary excretion pattern after repeated whole-body applications of a commercial sunscreen, containing 4% BZ-3, to 25 healthy volunteers. Methods Each sample was analyzed with regard to both conjugated/non-conjugated BZ-3 and conjugated/non-conjugated DHB, since both BZ-3 and DHB are extensively conjugated in the body. Solid-phase extraction (SPE) with C8 columns was followed by reverse-phase HPLC. For separation a Genesis C18 column was used with an acethonitrile-water mobile phase and the UV-detector was set at 287 nm. Results The assay was linear r 2 > 0.99, with detection limits for BZ-3 and DHB of 0.01 µmol L-1 and 0.16 µmol L-1 respectively. Relative standard deviation (RSD) was less than 10% for BZ-3 and less than 13% for DHB. The excretion pattern varied among the human volunteers; we discerned different patterns among the individuals. Conclusions The reverse-phase HPLC assay and extraction procedures developed are suitable for use when a large number of samples need to be analyzed and the method fulfilled our objectives. The differences in excretion pattern may be due to differences in enzyme activity but further studies, especially about genetic polymorphism, need to be performed to verify this finding.

scholarly journals Application of a Pillared-Layer Zn-Triazolate Metal-Organic Framework in the Dispersive Miniaturized Solid-Phase Extraction of Personal Care Products from Wastewater Samples

Molecules ◽  
2019 ◽  
Vol 24 (4) ◽  
pp. 690 ◽  
Author(s):  
Providencia González-Hernández ◽  
Ana Lago ◽  
Jorge Pasán ◽  
Catalina Ruiz-Pérez ◽  
Juan Ayala ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Metal Organic Framework ◽  
Personal Care Products ◽  
Aqueous Sample ◽  
Phase Extraction ◽  
Personal Care ◽  
Relative Standard ◽  
Metal Organic ◽  
Organic Framework

The pillared-layer Zn-triazolate metal-organic framework (CIM-81) was synthesized, characterized, and used for the first time as a sorbent in a dispersive micro-solid phase extraction method. The method involves the determination of a variety of personal care products in wastewaters, including four preservatives, four UV-filters, and one disinfectant, in combination with ultra-high performance liquid chromatography and UV detection. The CIM-81 MOF, constructed with an interesting mixed-ligand synthetic strategy, demonstrated a better extraction performance than other widely used MOFs in D-µSPE such as UiO-66, HKUST-1, and MIL-53(Al). The optimization of the method included a screening design followed by a Doehlert design. Optimum conditions required 10 mg of CIM-81 MOF in 10 mL of the aqueous sample at a pH of 5, 1 min of agitation by vortex and 3 min of centrifugation in the extraction step; and 1.2 mL of methanol and 4 min of vortex in the desorption step, followed by filtration, evaporation and reconstitution with 100 µL of the initial chromatographic mobile phase. The entire D-µSPE-UHPLC-UV method presented limits of detection down to 0.5 ng·mL−1; intra-day and inter-day precision values for the lowest concentration level (15 ng·mL−1)-as a relative standard deviation (in %)-lower than 8.7 and 13%, respectively; average relative recovery values of 115%; and enrichment factors ranging from ~3.6 to ~34. The reuse of the CIM-81 material was assessed not only in terms of maintaining the analytical performance but also in terms of its crystalline stability.

scholarly journals Syringe-Cartridge Solid-Phase Extraction Method for Patulin in Apple Juice

2003 ◽  
Vol 86 (6) ◽  
pp. 1160-1163 ◽  
Author(s):  
Thomas A Eisele ◽  
Midori Z Gibson
Keyword(s):  
Solid Phase Extraction ◽  
Apple Juice ◽  
Solid Phase ◽  
Potassium Phosphate ◽  
Test Sample ◽  
Reversed Phase ◽  
Phase Extraction ◽  
Relative Standard ◽  
Phase Liquid ◽  
Spe Method

Abstract A syringe-cartridge solid-phase extraction (SPE) method was developed for determination of patulin in apple juice. A 2.5 mL portion of test sample was passed through a conditioned macroporous SPE cartridge and washed with 2 mL 1% sodium bicarbonate followed by 2 mL 1% acetic acid. Patulin was eluted with 1 mL 10% ethyl acetate in ethyl ether and determined by reversed-phase liquid chromatography using a mobile phase consisting of 81% acetonitrile, 9% water, and 10% 0.05M potassium phosphate buffer, pH 2.4. Recoveries averaged 92% and the relative standard deviation was 8.0% in test samples spiked with 50 ng/mL patulin. The method appears to be applicable for monitoring apple juice samples to meet the U.S. Food and Drug Administration compliance action level of 50 μg/kg in an industrial quality assurance laboratory environment.

scholarly journals Solid-Phase Extraction Cleanup and Liquid Chromatography with Ultraviolet Detection of Ephedrine Alkaloids in Herbal Products

1998 ◽  
Vol 81 (6) ◽  
pp. 1121-1127 ◽  
Author(s):  
Jeffrey A Hurlbut ◽  
Justin R Carr ◽  
Emma R Singleton ◽  
Kent C Faul ◽  
Mark R Madson ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Phase Extraction ◽  
Isocratic Elution ◽  
Herbal Products ◽  
Ultraviolet Detection ◽  
Relative Standard ◽  
Triethyl Amine ◽  
Label Claim ◽  
Liquid Chromatographic

Abstract A solid-phase extraction (SPE) cleanup and a liquid chromatographic (LC) method with UV detection is presented for analysis of up to 7 ephedrine alkaloids in herbal products. Alkaloids from herbal products are extracted with acidified buffer, isolated on a propylsulfonic acid SPE column, eluted with a high-ionic-strength buffer, and separated by LC with detection at 255 nm. LC separation is performed by isocratic elution on a YMC phenyl column with 0.1 M sodium acetate-acetic acid (pH = 4.8) containing triethyl-amine and 2% acetonitrile. Ephedrine alkaloids are completely separated in 15 min. Average recovery of 5 common alkaloids from 3 spiked matrixes is 90%, with an average relative standard deviation (RSD) of 4.4% for alkaloid spikes between 0.5 and 16 mg/g. Average quantitation of ephedrine and pseudoephedrine from 6 herbal products is 97% of declared label claims, and average quantitation of synephrine from an herbal dietary product is 85% of label claim (RSD, 3.2%). Recoveries of synephrine, norephedrine, ephedrine, pseudoephedrine, N-methylephedrine, and N-methylpseudoephedrine spiked in 4 herbal products averaged 95%. Results of ruggedness testing and of a second laboratory validation of the procedure are also presented.

scholarly journals Novel Chromatographic Separation and Carbon Solid-Phase Extraction of Acetanilide Herbicide Degradation Products

2002 ◽  
Vol 85 (6) ◽  
pp. 1331-1337 ◽  
Author(s):  
Jody A Shoemaker
Keyword(s):  
Drinking Water ◽  
Solid Phase Extraction ◽  
Chromatographic Separation ◽  
Solid Phase ◽  
Degradation Products ◽  
The United States ◽  
Negative Ion ◽  
Phase Extraction ◽  
Herbicide Degradation ◽  
Relative Standard

Abstract One acetamide and 5 acetanilide herbicides are currently registered for use in the United States. Over the past several years, ethanesulfonic acid (ESA) and oxanilic acid (OA) degradation products of these acetanilide/acetamide herbicides have been found in U.S. ground waters and surface waters. Alachlor ESA and other acetanilide degradation products are listed on the U.S. Environmental Protection Agency's (EPA) 1998 Drinking Water Contaminant Candidate List. Consequently, EPA is interested in obtaining national occurrence data for these contaminants in drinking water. EPA currently does not have a method for determining these acetanilide degradation products in drinking water; therefore, a research method is being developed using liquid chromatography/negative ion electrospray/mass spectrometry with solid-phase extraction (SPE). A novel chromatographic separation of the acetochlor/alachlor ESA and OA structural isomers was developed which uses an ammonium acetate–methanol gradient combined with heating the analytical column to 70°C. Twelve acetanilide degradates were extracted by SPE from 100 mL water samples using carbon cartridges with mean recoveries &gt;90% and relative standard deviations ≤16%.

scholarly journals Determination of Organic Acids in Salicornia herbacea by Solid-phase Extraction Combined with Liquid Chromatography

2013 ◽  
Vol 8 (2) ◽  
pp. 1934578X1300800
Author(s):  
Damian Han ◽  
Minglei Tian ◽  
Dong Wha Park ◽  
Kyung Ho Row
Keyword(s):  
Solid Phase Extraction ◽  
Ferulic Acid ◽  
Caffeic Acid ◽  
Solid Phase ◽  
Phase Extraction ◽  
Relative Standard ◽  
Trifluoracetic Acid ◽  
Spe Method ◽  
Salicornia Herbacea

A solid-phase extraction (SPE) method for the determination of procatechuic acid, ferulic acid and caffeic acid in Salicornia herbacea L. (Hamcho) has been developed. The optimal conditions were obtained by using a C18 SPE cartridge. By using ethanol and acetonitrile /water/ trifluoracetic acid as washing and eluting solvents, most interfering compounds originating from the hamcho matrix were eliminated. The extracts were sufficiently clean to be directly injected into the HPLC for further chromatographic analysis. Good linearity was obtained from 0.1 to 200 μg/mL (r > 0.999) for procatechuic acid, 0.2 to 400 μg/mL (r > 0.999) for caffeic acid and 0.3 to 600 μg/mL (r > 0.999) for ferulic acid, with the relative standard deviations being less than 3.6%. The mean recoveries of procatechuic acid, ferulic acid and caffeic acid from hamcho were more than 79.2% and the detection limit (S/N = 3:1) was 0.02 μg/mL for procatechuic acid, 0.01 μg/mL for caffeic acid and 0.04 μg/mL for ferulic acid. This method is a viable alternative to the existing HPLC methods for analyzing the content of procatechuic acid, ferulic acid and caffeic acid in hamcho.

The Determination of Eight Pesticides in Panax notoginseng of Chinese Traditional Medicine Using Solid-Phase Extraction and Gas Chromatography-Mass Spectrometry

2012 ◽  
Vol 485 ◽  
pp. 68-71
Author(s):  
Na Wu ◽  
Yu Da Zhang ◽  
Wei Liu ◽  
Ping Yi ◽  
Ze Feng Wang ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Panax Notoginseng ◽  
Gas Chromatography Mass Spectrometry ◽  
Phase Extraction ◽  
Selected Ion Monitoring ◽  
Chromatography Mass Spectrometry ◽  
Relative Standard

A simple and effective extraction method based on solid-phase extraction (SPE) was developed to determine chlorothalonil, metalaxyl, triadimefon, dimetachlone, procymidone, flumetralin, oxadixyl and iprodione in Panax Notoginseng using gas chromatography-mass spectrometry with selected ion monitoring (GC/MS, SIM). The prepared samples were analysed with GC-MS in the selected ion monitoring mode (SIM) using one target and two or three qualitative ions for each analyte. In the method, hexane - dichloromethane（6:4，v/v）was selected to effectively extract the pesticides from the Panax Notoginseng samples. Solid-phase extraction was carried out using Supelclean ENVI-Carb/NH2 SPE Column with acetonitrile-toluene (3:1, v/v) as the eluted solvent. In the linear range of each pesticide, the correlation coefficient was R2≥0.99. The limit of detection ranged from 0.001 to 0.05 µg.mL-1, average recoveries ranged from 79.80% to 95.00%, with relative standard deviations between 1.96% and 4.32% for all 8 pesticides.They were readily achieved with this method for all tested pesticides.

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