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

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.

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Spectrophotometric Determination of Iron(II) after Solid Phase Extraction of Its 2,2′ Bipyridine Complex on Silica Gel-Polyethylene Glycol

Journal of Spectroscopy ◽

10.1155/2013/548345 ◽

2013 ◽

Vol 2013 ◽

pp. 1-6 ◽

Cited By ~ 7

Author(s):

Nahid Pourreza ◽

Saadat Rastegarzadeh ◽

Ali Reza Kiasat ◽

Hossein Yahyavi

Keyword(s):

Polyethylene Glycol ◽

Solid Phase Extraction ◽

Silica Gel ◽

Limit Of Detection ◽

Solid Phase ◽

Extraction Procedure ◽

Calibration Graph ◽

Phase Extraction ◽

Relative Standard

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.

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Application of micro-nanostructured magnetite in separating tetrabromobisphenol A and hexabromocyclododecane from environmental water by magnetic solid phase extraction

PLoS ONE ◽

10.1371/journal.pone.0251021 ◽

2021 ◽

Vol 16 (5) ◽

pp. e0251021

Author(s):

Xiaoping Wang ◽

Fengzhi He ◽

Limin Zhang ◽

Ang Yu

Keyword(s):

Solid Phase Extraction ◽

Limit Of Detection ◽

Solid Phase ◽

Magnetic Solid Phase Extraction ◽

Environmental Water ◽

Mass Spectrometry Analysis ◽

Tetrabromobisphenol A ◽

Phase Extraction ◽

Relative Standard ◽

Magnetic Solid

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.

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Preparation of Polyphenol-Coated CoFe2O3 Nanoparticles for Magnetic Solid-Phase Extraction and Preconcentration of Lawsone by High-Performance Liquid Chromatography – DAD

10.20944/preprints202009.0668.v1 ◽

2020 ◽

Author(s):

Hassan Arkaban ◽

Mohammad Mirzaei ◽

Mansoreh Behzadi

Keyword(s):

Solid Phase Extraction ◽

Limit Of Detection ◽

Solid Phase ◽

Oxidative Polymerization ◽

Magnetic Solid Phase Extraction ◽

Polymerization Process ◽

Phase Extraction ◽

Extraction Temperature ◽

Relative Standard ◽

Magnetic Solid

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.

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Determination of 24 Pesticides Residues in Leather Products by Solid-Phase Microextraction Coupled with Gas Chromatography–Mass Spectrometry

Leather and Footwear Journal ◽

10.24264/lfj.20.4.5 ◽

2020 ◽

Vol 20 (4) ◽

pp. 385-404

Author(s):

Jinlan DAI ◽

Honglei YIN ◽

Hang WEI ◽

Lei ZHOU ◽

Minghua LIU

Keyword(s):

Mass Spectrometry ◽

Gas Chromatography ◽

Solid Phase Extraction ◽

Solid Phase ◽

Extraction Column ◽

Phase Extraction ◽

Mixed Solution ◽

Pesticides Residues ◽

Solid Phase Extraction Column ◽

Relative Standard

Considering the high content of oil and complex residual additives in leather samples, a new analytical method based on the solid-phase extraction technique and gas chromatography-selected ion monitoring mass spectrometry (GC-SIM-MS) was developed to determine 24 organic compounds involving the organochlorine pesticides (OCPs), organophosphorous pesticides (OPPs) and pyrethroids pesticides residues in leather. The extraction conditions (such as the extraction solution, purification procedure and solid-phase extraction column) were optimized using the positive leather samples based on the recovery rates of the pesticides. The best extraction solution, solid-phase extraction column and chromatography column were n-hexane and ethyl acetate (1+1, volume) mixed solution, Carb-PSA (1.0 g, 6mL) and DB-1701 (length: 30 m, inside diameter: 0.25 mm, film thickness: 0.25 μm). The optimized extraction time and temperature were 20 min and 25°C, respectively. The detection limits of 24 pesticide residues range from 0.05 to 0.10 mg/kg, and the recoveries range from 74% to 116%. The relative standard deviations (RSD, n=6) range from 5.42% to 12.00%. The developed method presented a simple, rapid, sensitive, and inexpensive method to detect 24 pesticides in skin and leather and was successfully applied to the detect them in leather products (cowhide, sheep leather and pig leather).

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Determination of Imazaquin Residues in Soil by Solid-Phase Extraction and High-Performance Liquid Chromatography

Journal of AOAC International ◽

10.1093/jaoac/90.2.568 ◽

2007 ◽

Vol 90 (2) ◽

pp. 568-574 ◽

Cited By ~ 4

Author(s):

Chen Xuyan ◽

Hu Jiye ◽

Li Jianzhong

Keyword(s):

High Performance Liquid Chromatography ◽

Liquid Chromatography ◽

Solid Phase Extraction ◽

High Performance ◽

Limit Of Detection ◽

Solid Phase ◽

Phase Extraction ◽

Application Rates ◽

Relative Standard ◽

Strong Anion Exchange

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.

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Multiresidue Determination of Pesticides in Drinking and Related Waters by Solid-Phase Extraction and Liquid Chromatography with Ultraviolet Detection: Interlaboratory Study

Journal of AOAC International ◽

10.1093/jaoac/85.2.375 ◽

2002 ◽

Vol 85 (2) ◽

pp. 375-383 ◽

Cited By ~ 2

Author(s):

François van Hoof ◽

Peter van Wiele ◽

Françoise Acobas ◽

Jean-Luc Guinamant ◽

Auguste Bruchet ◽

...

Keyword(s):

Liquid Chromatography ◽

Standard Deviation ◽

Solid Phase Extraction ◽

Relative Standard Deviation ◽

Limit Of Detection ◽

Solid Phase ◽

Tap Water ◽

Phase Extraction ◽

Relative Standard ◽

Styrene Divinylbenzene

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%.

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Multi Mycotoxins Analysis in Rice Using LC-MS/MS

Media Pharmaceutica Indonesiana (MPI) ◽

10.24123/mpi.v1i2.189 ◽

2017 ◽

Vol 1 (2) ◽

pp. 77-84

Author(s):

Riswahyuli Riswahyuli ◽

Loise RS ◽

Niza Nemara

Keyword(s):

Solid Phase Extraction ◽

Limit Of Detection ◽

Solid Phase ◽

Extraction Column ◽

Phase Extraction ◽

Accurate Data ◽

Develop Method ◽

Limit Of Quantification ◽

Novel Technology ◽

Aflatoxin B2

Multi mycotoxins analysis in this research has the purpose to develop method of analysisfor rice sample with a simple and fast preparation and novel technology using LC-MS/MS. Several blankrice samples were spiked with standards of 8 classes of mycotoxins (Aflatoxin B1, Aflatoxin B2, AflatoxinG1, Aflatoxin G2, Deoxynivalenol, Zearalenon, T-2, and HT-2). Parameter of linearity, precision, recovery,limit of detection and limit of quantification were obtained and calculated. The result shows that all thevalidation parameters comply with criteria of method validation. Sonication method that was chosen toextract analites and Solid Phase Extraction Column that used for sample clean up are successful methodsthat have contribution for precise and accurate data. The Identification and quantification with LC-MS/MS help to determine and distinguish each mycotoxin through chromatogram appearance, retention timeand a specific m/z.

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Amino-Functionalization of Multiwall Carbon Nanotubes and Its Use for Solid Phase Extraction of Mercury Ions from Fish Sample

ISRN Nanotechnology ◽

10.1155/2013/674289 ◽

2013 ◽

Vol 2013 ◽

pp. 1-8 ◽

Cited By ~ 13

Author(s):

Majid Soleimani ◽

Majid Ghahraman Afshar ◽

Arman Sedghi

Keyword(s):

Carbon Nanotubes ◽

Solid Phase Extraction ◽

Limit Of Detection ◽

Solid Phase ◽

Multiwall Carbon Nanotubes ◽

Phase Extraction ◽

Relative Standard ◽

Amino Functionalization ◽

Functionalized Mwcnts ◽

Multiwall Carbon

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+.

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Survey of Octylphenol, Nonylphenol, and Bisphenol A in Infant Milk Powders by Solid-Phase Extraction Combined GC/MS Method

Journal of Food Quality ◽

10.1155/2018/2848627 ◽

2018 ◽

Vol 2018 ◽

pp. 1-8

Author(s):

Chenggang Cai ◽

Yibin Ying ◽

Pinggu Wu ◽

Jun Tang ◽

Liyuan Wang ◽

...

Keyword(s):

Bisphenol A ◽

Solid Phase Extraction ◽

Endocrine Disruptors ◽

Limit Of Detection ◽

Solid Phase ◽

Milk Powder ◽

Phase Extraction ◽

Relative Standard ◽

Limit Of Quantitation ◽

Infant Milk Powder

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.

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Solid-Phase Extraction and Spectrophotometric Determination of Iodate in Table Salt after Azo Dye Formation

Journal of AOAC International ◽

10.1093/jaoac/82.1.167 ◽

1999 ◽

Vol 82 (1) ◽

pp. 167-171 ◽

Cited By ~ 2

Author(s):

Shefali Gosain ◽

Madhurima Pandey ◽

Krishna K Verma

Keyword(s):

Solid Phase Extraction ◽

Azo Dye ◽

Limit Of Detection ◽

Solid Phase ◽

Molar Absorptivity ◽

Calibration Graph ◽

Phase Extraction ◽

Table Salt ◽

Acid Cation

Abstract A new reaction for determining iodate in table salt is proposed. It is based on oxidation of phenylhy-drazine-4-sulfonic acid by iodate in acidic medium to the 4-diazobenzenesulfonic acid cation and its electrophilic coupling with N-(1-naphthyl)ethylene- diamine dihydrochloride to give an azo dye, which is measured spectrophotometrically at 545 nm. Maximum molar absorptivity was 8.41 ×104 L/mol cm. A rectilinear calibration graph was obtained for iodate in the range 0.25–5 mg/L. The azo dye could be preconcentrated at least 40-fold by solid-phase extraction on C18 sorbent. The limit of detection was 0.6 μg iodate/L. The method was used to determine iodate in laboratory-prepared and commercially available table salt samples. Up to 5 mg bromate/kg and 10 mg iron(lll)/kg in table salt did not interfere.

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