scholarly journals Development of a Disposable Pipette Extraction Method Using Coffee Silverskin as an Adsorbent for Chromium Determination in Wastewater Samples by Solid Phase Extraction

Author(s):  
Weida Silva ◽  
Bruno Costa ◽  
Alex Batista ◽  
Vanessa Alves ◽  
Nivia Coelho

A procedure using disposable pipette tips adapted for solid-phase extraction, known as DPX‑SPE, was used as an alternative way for the chromium determination in wastewater samples. DPX-SPE consists of a device which allows a dynamic contact between the sample and the solidphase. A residue obtained from the processing of coffee beans, denominate coffee silverskin, was used as a new adsorbent. Characterization techniques revealed properties of lignocellulosic materials with potential application for chromium adsorption. The parameters including adsorbent mass (25.00 mg), elution solvent (0.1 mol L−1 HCl, 200 μL) and pH (2.0) were optimized. Thus, 1.00 mL of deionized water for conditioning, 4.00 mL of sample, 2 extraction cycles and 1 elution cycle were the employed conditions. Enrichment factor of 12, limit of detection of 6.00 μg L−1 and relative standard deviation (RSD) 1.3% (n = 3) were obtained. The method proved to be fast, cheap, environmentally friendly, and simple, providing good recoveries (104-113%), and it was satisfactorily applied in real samples.

2011 ◽  
Vol 89 (4) ◽  
pp. 517-523 ◽  
Author(s):  
Ke-Jing Huang ◽  
Cong-Hui Han ◽  
Ying-Ying Wu ◽  
Chao-Qun Han ◽  
De-Jun Niu ◽  
...  

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.


2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Nahid Pourreza ◽  
Saadat Rastegarzadeh ◽  
Ali Reza Kiasat ◽  
Hossein Yahyavi

A new solid phase extraction procedure was developed for preconcentration of iron(II) using silica gel-polyethylene glycol (silica-PEG) as an adsorbent. The method is based on retention of iron(II) as 2,2′ bipyridine complex on silica-PEG. The retained complex is eluted by 1.0 mol L−1of sulfuric acid-acetone mixture (1:2) and its absorbance is measured at 518 nm, spectrophotometrically. The effects of different parameters such as pH, concentration of the reagent, eluting reagent, sample volume, amount of adsorbent, and interfering ions were investigated. The calibration graph was linear in the range of 1–60 ng mL−1of iron(II). The limit of detection based on3Sbwas 0.57 ng mL−1and relative standard deviations (R.S.D) for ten replicate measurements of 12 and 42 ng mL−1of iron(II) were 2.4 and 1.7%, respectively. The method was applied to the determination of of iron(II) in water, multivitamin tablet, and spinach samples.


PLoS ONE ◽  
2021 ◽  
Vol 16 (5) ◽  
pp. e0251021
Author(s):  
Xiaoping Wang ◽  
Fengzhi He ◽  
Limin Zhang ◽  
Ang Yu

Two typical brominated flame retardants (BFRs), namely, tetrabromobisphenol A (TBBPA) and hexabromocyclododecane (HBCD), were persistent organic pollutants widely detected in various environmental media. This study aimed to successfully synthesize micro-nano-structured magnetite particles (MNMPs) with surface modification by citric acid molecules. The synthesized composites served as an adsorbent for extracting TBBPA and HBCD from environmental water samples followed by gas chromatography–mass spectrometry analysis. The obtained MNMPs were characterized in terms of crystal structure, morphology, size distribution, hydrophobic and hydrophilic performance and magnetism. The results indicated that the MNMPs exhibited high surface area, good dispersibility, and strong magnetic responsiveness for separation. The parameters affecting the extraction efficiency were optimized, including sample pH, amount of sorbents, extraction time and desorption conditions. Under the optimum conditions, the recovery was 83.5 and 107.1%, limit of detection was 0.13 and 0.35μg/mL (S/N = 3), and limit of quantification was 0.37 and 0.59 μg/mL (S/N = 10) for TBBPA and HBCD respectively. The relative standard deviations obtained using the proposed method were less than 8.7%, indicating that the MNMP magnetic solid-phase extraction method had advantages of simplicity, good sensitivity and high efficiency for the extraction of the two BFRs from environmental water.


Author(s):  
Hassan Arkaban ◽  
Mohammad Mirzaei ◽  
Mansoreh Behzadi

A novel polyphenol‑coated CoFe2O4 system was synthesized as a magnetic adsorbent by chemical oxidative polymerization process for magnetic solid-phase extraction of lawsone. The synthesized nanoadsorbent showed a spherical morphology with diameters under 50 nm by scanning electron microscopy images. The extraction efficiency of this adsorbent was studied towards the extraction of lawsone from saline aqueous solution in dispersion mode. Major parameters including the type and volume of desorption solvent, amount of sorbent, desorption time, extraction time, extraction temperature, ionic strength and pH were optimized. Under the optimum conditions the relative standard deviation in 0.005 µg mL-1 (inter-day n = 6; intra-day: n = 6; and adsorbent to adsorbent n = 4) were obtained as 5.2, 8.07 and 11.7%, respectively. A linear calibration curve in the range of 0.003–0.5 µg mL-1 with R2 = 0.993 was obtained. The limit of detection and limit of quantification of the method were 0.001 µg mL-1 and 0.003 µg mL-1, respectively. The relative recovery percentages were in range of 90-96.4% for henna leaves, henna shampoo, and henna dermal lotion real samples.


2007 ◽  
Vol 90 (2) ◽  
pp. 568-574 ◽  
Author(s):  
Chen Xuyan ◽  
Hu Jiye ◽  
Li Jianzhong

Abstract A method has been developed for the quantitation of imazaquin residues in soil. The herbicide was extracted from soil with methanolwater (2 + 1, v/v) and cleaned up by strong anion-exchange solid-phase extraction cartridges. Analysis was performed by using high-performance liquid chromatography with ultraviolet detection. Average recoveries through the method ranged from 90.7 to 100.6%, with relative standard deviation equal to or lower than 6.6%. The limit of detection was estimated to be 0.0015 mg/kg, and the minimum quantitation concentration of imazaquin in soil was 0.005 mg/kg. This method was successfully applied to evaluate imazaquin residue levels in soil and its dissipation rates in a soybean field in the Xisanqi District of Beijing, People's Republic of China. The dissipation study showed that the half life of imazaquin in soil was 10.37 0.0135 days at 3 different application rates.


2002 ◽  
Vol 85 (2) ◽  
pp. 375-383 ◽  
Author(s):  
François van Hoof ◽  
Peter van Wiele ◽  
Françoise Acobas ◽  
Jean-Luc Guinamant ◽  
Auguste Bruchet ◽  
...  

Abstract As part of a project funded by the European Commission (EC) for the development and evaluation of multiresidue methods for analysis of drinking and related waters, 17 European laboratories evaluated a method using styrene–divinylbenzene copolymer solid-phase extraction followed by liquid chromatography with diode array detection. The main aim of the study was to evaluate whether the method meets the requirements of EC Drinking Water Directive 98/83 in terms of accuracy, precision, and detection limit for 21 pesticides according to the following requirements: limit of detection, ≤0.025 μg/L; accuracy expressed as recovery, between 75 and 125%; and precision expressed as repeatability relative standard deviation of the method, <12.5%, and as reproducibility relative standard deviation of the method, <25%. Analyses for unknown concentrations were performed with commercial bottled and tap waters. All laboratories were able to achieve detection limits of 0.01 μg/L for all pesticides except pirimicarb (0.02 μg/L). The criteria for repeatability were met for all compounds. Terbutryn in bottled water and carbendazim in tap water did not meet the criteria for reproducibility. In terms of accuracy, the method met the requirements for all pesticides in both matrixes, except for metamitron. However, several compounds (linuron, terbutryn, propazine, metobromuron, and isoproturon) showed recoveries slightly below 75%.


2013 ◽  
Vol 2013 ◽  
pp. 1-8 ◽  
Author(s):  
Majid Soleimani ◽  
Majid Ghahraman Afshar ◽  
Arman Sedghi

We describe here the amino-functionalization of multiwall carbon nanotubes (MWCNTs) and also its application as an adsorbent of solid phase extraction (SPE). The amino-functionalized MWCNTs have a good capacity to retain Hg2+, but the raw and purified MWCNTs are found not to adsorb Hg2+ ions. The amino-functionalized MWCNTs are prepared with amino-functionalization of purified MWCNTs by ethylenediamine. The physicochemical properties of purified and amino-functionalized MWCNTs are characterized by Fourier transform infrared spectroscopy, thermogravimetric analysis, and the Boehm titration. The amino-functionalized MWCNTs are selected as novel sorbents for the solid phase extraction of Hg2+. The amino-functionalized MWCNT-SPE method is used for the determination of Hg2+ from complex matrix including fish and real water samples. Effective parameters on Hg2+ retention such as pH, flowrate, nature of the eluent, the ionic strength, selectivity coefficient, and retention capacity are investigated. The enrichment factor and maximum capacity of the sorbent are 100 mL and 11.58 mg/g, respectively. The linear range, limit of detection, and relative standard deviation of the proposed method are 0.003 to 0.3 μg/L, 1.25×10−3 μg/L, and 2.23%, respectively. Selectivity experiments show that the adsorbents have a stronger specific retention for Hg2+ than Fe3+, Cu2+, Pb2+, Ni2+, Mn2+, Ca2+, and Mg2+.


2018 ◽  
Vol 2018 ◽  
pp. 1-8
Author(s):  
Chenggang Cai ◽  
Yibin Ying ◽  
Pinggu Wu ◽  
Jun Tang ◽  
Liyuan Wang ◽  
...  

A detection method for 3 kinds of phenolic compounds of endocrine disruptors (4-nonylphenol, 4-octylphenol, and bisphenol A) in infant milk powders by solid-phase extraction combined GC-MS was established. This method can effectively remove interference materials from infant milk powder products. The limit of detection and the limit of quantitation of the 3 kinds of compounds were 0.8 μg/kg and 2.5 μg/kg, respectively, with the relative standard deviations of 4.3–12.1%. The recovery rates of 4-nonylphenol, 4-octylphenol, and bisphenol A were of 68.5–89.2%, 64.8–87.0%, and 97.8–110.0%, respectively. Concentrations of the bisphenol A were from 0.8 to 14 μg/kg in 35 samples of the total 60 samples. And the other two compounds of 4-nonylphenol and 4-octylphenol were not found in all the 60 samples tested. The established method is simple, rapid, accurate, and highly sensitive, and the pollution of endocrine disruptors in some infant milk powders products was detectable in trace amounts.


2012 ◽  
Vol 9 (3) ◽  
pp. 1550-1561 ◽  
Author(s):  
Saksit Chanthai ◽  
Jureerat Juangsamoot ◽  
Chalerm Ruangviriyachai ◽  
Suchila Techawongstien

Reversed phase-HPLC with fluorescence detection of two major capsaicinoids was described. Isocratic elution using a ratio of methanol and deionized water (66:34, v/v) as mobile phase was used at a flow rate of 0.9 mL/min with well achieved separation within 6 min. Under optimum conditions, their analytical figures of merit for the HPLC method were validated. The linearity was in the range of 1.0-25.0 μg/mL with multiple determination coefficients of higher than 0.995. The limit of detection was ranged of 0.008-0.01 μg/mL. The repeatability and reproducibility of the retention time and peak area for these compounds were in good precision with their relative standard deviations (RSDs) lower than 1% and 5%, respectively. Both capsaicin and dihydrocapsaicin were extracted using an accelerated solvent extraction (ASE) of methanol as an extraction solvent for 5 min static time with 3 cycles. The methanolic extracts were subjected to clean up with C18solid-phase extraction (SPE) with its recoveries ranking of 90.2-98.0%. The method recoveries of real samples were found to be 60.7-98.6%. The optimized extraction method were applied for the determination of the two capsaicinoids in ten vareities of hot chilli pepper samples. Total contents of capsaicinoids were found in the range of 2,307.0-9047.3 μg/g DW with their corresponding Scoville heat unit (SHU) of 34,600-135,700. Additionally, the contents of capsaicinoids using external calibration method comparing with those of standard addition were not significantly different, indicating accuracy of the method. Mostly, the contents of capsaicin found in these real samples were rather higher than those of dihydrocapsaicin.


2018 ◽  
Vol 77 (9) ◽  
pp. 2220-2227 ◽  
Author(s):  
Guo Li ◽  
Ruoyu Deng ◽  
Guilong Peng ◽  
Chun Yang ◽  
Qiang He ◽  
...  

Abstract Magnetic Fe3O4 graphene oxide nanocomposite was synthesized by chemical coprecipitation method and characterized by scanning electron microscopy, Fourier transform infrared spectra and X-ray diffraction. A simple, rapid, convenient and environmentally friendly method was developed for separation and pre-concentration of trace amounts of bisphenol A, naproxen and triclosan in wastewater samples by high performance liquid chromatography with magnetic Fe3O4 graphene oxide nanocomposite as the adsorbent for magnetic solid-phase extraction. Various parameters possibly influencing the extraction performance such as amount of the adsorbent, extraction time, sample pH and elution conditions were optimized. Under the optimal working conditions, the developed method showed good linearity (R > 0.9997) in the range of 1–200 μg/L, and the limits of detection are between 0.5 and 0.8 μg/L. The enrichment factors are in the range of 81–89. The repeatability of the method, expressed as relative standard deviation, is 3.36–4.26%.


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