Chromatographic Determination of Total Selenium in Biofortified Allium sp. following Piazselenol Formation and Micro-Solid-Phase Extraction

Herein, a method based on selective piazselenol formation is applied for total selenium determination in biofortified Allium species. Piazselenol is formed by reacting Se(IV) with an aromatic diamine, namely 4-nitro-1,2-phenylenediamine, in acidic medium. Samples were digested in a nitric acid/hydrogen peroxide open system, followed by selenate reduction in hydrochloric acid. Reaction conditions were optimized in terms of pH, temperature, reaction time, and other auxiliary reagents for interference removal, namely, EDTA and hydroxylamine. For the extraction of the selectively formed 4-nitro-piazselenol, micro-solid-phase extraction (μSPE) was applied, and the analysis and detection of the corresponding complex was performed by HPLC coupled with DAD. An external standard calibration curve was developed (R2 = 0.9994) with good sensitivity, and was used to calculate the total selenium content from several Allium plants material, with good intermediate precision (RSD% < 16%). The accuracy of the method was evaluated using both, a comparison with an accepted reference method from our previously published data, as well as three certified reference material with recoveries between 84–126%. The limit of detection was determined to be 0.35 μg/g (in solids) and 1.1 μg/L (in solution), while the limit of quantification was 1.07 μg/g and 3.4 μg/L (in solution). Using the proposed method, selenium content can be quickly and accurately determined in several types of samples. In addition, this study present experimental conditions for overcoming the interferences that might be encountered in selenium determination using piazselenol.

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

Canadian Journal of Chemistry ◽

10.1139/v11-006 ◽

2011 ◽

Vol 89 (4) ◽

pp. 517-523 ◽

Cited By ~ 2

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.

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Greener Monolithic Solid Phase Extraction Biosorbent Based on Calcium Cross-Linked Starch Cryogel Composite Graphene Oxide Nanoparticles for Benzo(a)pyrene Analysis

Molecules ◽

10.3390/molecules26206163 ◽

2021 ◽

Vol 26 (20) ◽

pp. 6163

Author(s):

Aree Choodum ◽

Nareumon Lamthornkit ◽

Chanita Boonkanon ◽

Tarawee Taweekarn ◽

Kharittha Phatthanawiwat ◽

...

Keyword(s):

Graphene Oxide ◽

Solid Phase Extraction ◽

Limit Of Detection ◽

Solid Phase ◽

High Sensitivity ◽

Rice Flour ◽

Oxide Nanoparticles ◽

Phase Extraction ◽

Limit Of Quantification ◽

Significant Difference

Benzo(a)pyrene (BaP) has been recognized as a marker for the detection of carcinogenic polycyclic aromatic hydrocarbons. In this work, a novel monolithic solid-phase extraction (SPE) sorbent based on graphene oxide nanoparticles (GO) in starch-based cryogel composite (GO-Cry) was successfully prepared for BaP analysis. Rice flour and tapioca starch (gel precursors) were gelatinized in limewater (cross-linker) under alkaline conditions before addition of GO (filler) that can increase the ability to extract BaP up to 2.6-fold. BaP analysis had a linear range of 10 to 1000 µgL−1 with good linearity (R2 = 0.9971) and high sensitivity (4.1 ± 0.1 a.u./(µgL−1)). The limit of detection and limit of quantification were 4.21 ± 0.06 and 14.04 ± 0.19 µgL−1, respectively, with excellent precision (0.17 to 2.45%RSD). The accuracy in terms of recovery from spiked samples was in the range of 84 to 110% with no significant difference to a C18 cartridge. GO-Cry can be reproducibly prepared with 2.8%RSD from 4 lots and can be reused at least 10 times, which not only helps reduce the analysis costs (~0.41USD per analysis), but also reduces the resultant waste to the environment.

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Magnetically responsive materials for solid phase extraction

Environmental engineering ◽

10.37023/ee.6.1.3 ◽

2019 ◽

Vol 6 (1) ◽

pp. 15-20 ◽

Cited By ~ 3

Author(s):

Ivo Safarik ◽

Jitka Prochazkova ◽

Eva Baldikova ◽

Kristyna Pospiskova

Keyword(s):

Solid Phase Extraction ◽

Limit Of Detection ◽

Solid Phase ◽

Analytical Techniques ◽

Magnetic Solid Phase Extraction ◽

Short Review ◽

Biologically Active ◽

Phase Extraction ◽

Responsive Materials ◽

Magnetic Solid

Magnetically responsive materials have found many important applications in analytical chemistry. In this short review the basic information about Magnetic solid phase extraction and Magnetic textile solid phase extraction is given. These analytical techniques enable to preconcentrate target biologically active compounds or pollutants from water samples. Both procedures enable to lower the limit of detection using conventional analytical procedures.

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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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Development and Validation of RP-HPLC Method for Azilsartan Medoxomil Potassium Quantitation in Human Plasma by Solid Phase Extraction Procedure

ISRN Spectroscopy ◽

10.1155/2013/572170 ◽

2013 ◽

Vol 2013 ◽

pp. 1-6 ◽

Cited By ~ 4

Author(s):

Paras P. Vekariya ◽

Hitendra S. Joshi

Keyword(s):

Solid Phase Extraction ◽

Human Plasma ◽

Limit Of Detection ◽

Solid Phase ◽

Hplc Method ◽

Array Detector ◽

Phase Extraction ◽

Rp Hplc ◽

Limit Of Quantitation ◽

Azilsartan Medoxomil

Simple and rapid reverse phase high-performance liquid chromatography (RP-HPLC) method was developed and validated using solid phase extraction (SPE) technique for the determination of Azilsartan Medoxomil Potassium (AMP) in human plasma; detection was carried out by photo diode array detector. Chromatographic separation of the analyte AMP was achieved within 7.5 min by Waters symmetry C18 (4.6 × 250 mm, 5 µm) column, mobile phase was 25 mM ammonium acetate buffer (pH 5.5): acetonitrile 55 : 45 v/v, flow rate was 1.0 mL/min, and the detection was carried out at 254 nm. Calibration curve was linear (r2 > 0.9985) in the range of 1.0–9.0 µg/mL, limit of detection (LOD) and limit of quantitation (LOQ) were 0.150 µg/mL and 0.400 µg/mL, respectively, and intra- and interday deviations were between 1.53–8.41% and 1.78–4.59%, respectively. The overall mean recovery of AMP was 92.35%. No any endogenous constituents were found to interfere at retention time of the analyte. This new RP-HPLC method was successfully validated and may be applied to conduct bioavailability and bioequivalence studies of AMP.

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Adsorption of Organic Pollutants in Wastewater using Solid Phase Extraction Absorbent from Agro-Waste

Current Agriculture Research Journal ◽

10.12944/carj.7.2.12 ◽

2019 ◽

Vol 7 (2) ◽

pp. 245-253 ◽

Cited By ~ 1

Author(s):

Wan Norfazilah Wan Ismail ◽

Dzul Iskandar Muhammad Fauzi ◽

Nurlin Abu Samah

Keyword(s):

Solid Phase Extraction ◽

Organic Pollutants ◽

Limit Of Detection ◽

Solid Phase ◽

Sample Volume ◽

Wastewater Sample ◽

Phase Extraction ◽

Nano Powder ◽

Optimum Parameters ◽

Limit Of Quantitation

A rapid solid phase extraction (SPE) combined with gas chromatography equipped with mass spectrometry (GC-MS) method was developed and validated for the determination of acenaphthylene, acenaphthene and naphthalene in wastewater sample collected from petroleum industry’s drainage. Important SPE parameters, namely absorbent amount, sample volume, type of elution solvent and its volume were optimized. The optimum parameters obtained are: 200 mg silica nano-powder, 2.0 mL sample volume and 2.0 mL n-hexane as elution solvent. The method showed good linearity in the range of 0.1-10.0 mg/L with satisfactory limit of detection (≤1.0 mg/L) and limit of quantitation (≤3.2 mg/L) under the optimized conditions. Good relative recoveries (94.7-99.9%) and intra- and inter-day precisions (≤2.8%, n=3) for acenaphthene, acenaphthylene and naphthalene were obtained. Toxicity study has revealed that it is a non-toxic absorbent and safe to be used for the removal of organic pollutants in water which is advantageous for routine wastewater analysis.

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Presence of zearalenone in the most commonly grown wheat cultivars in Serbia

Zbornik Matice srpske za prirodne nauke ◽

10.2298/zmspn1324101j ◽

2013 ◽

pp. 101-109 ◽

Cited By ~ 1

Author(s):

Igor Jajic ◽

Sasa Krstovic ◽

Biljana Perisic ◽

Sandra Jaksic ◽

Vojislava Bursic ◽

...

Keyword(s):

Liquid Chromatography ◽

Solid Phase Extraction ◽

Limit Of Detection ◽

Solid Phase ◽

Phase Extraction ◽

Wheat Cultivars ◽

Limit Of Quantification ◽

Average Value ◽

Contamination Levels ◽

Maximum Limit

A total of 45 samples of wheat from three different locations in Vojvodina were analyzed for the presence of zearalenone. Analytical methods based on clean-up by solid-phase extraction (SPE) columns and detection by liquid chromatography were used after validation. Limit of detection for ZEA in wheat was 18.6 ?g/kg and the limit of quantification was 56.5 ?g/kg. Recovery values ranged between 86% and 97%. The occurrence of ZEA in wheat was rather high with 53.3% of positive samples with the average value of 330 ?g/kg. Incidences were found from 68 ?g/kg to 1079 ?g/kg. Contamination levels were above the established maximum limit for unprocessed cereals, other than maize, in as many as seventeen samples. These results were compared to the results of investigation of deoxynivalenol and fumonisin content, established in our previous work on the same samples. The results obtained were also compared to those of the neighboring countries where the relevant data existed and to the data of previous studies in our country.

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Determination of Phthalate Plasticisers in Palm Oil Using Online Solid Phase Extraction-Liquid Chromatography (SPE-LC)

Journal of Chemistry ◽

10.1155/2014/682975 ◽

2014 ◽

Vol 2014 ◽

pp. 1-9 ◽

Cited By ~ 5

Author(s):

Nazarudin Ibrahim ◽

Rozita Osman ◽

Azmui Abdullah ◽

Norashikin Saim

Keyword(s):

Solid Phase Extraction ◽

Palm Oil ◽

Limit Of Detection ◽

Solid Phase ◽

Correlation Coefficients ◽

Array Detector ◽

Phase Extraction ◽

Extraction Solvent ◽

Online Solid Phase Extraction

Contamination of phthalates plasticisers to food has raised concern as some of the phthalates are suspected to be endocrine disruptors. The phthalates have high affinity with oily environment and analysing these chemicals in such matrices is difficult because of the trace amount of the analyte and interference from matrix. An online solid phase extraction (SPE) technique using a large volume (3.5 mL) injection was developed for the analysis of 6 common plasticisers in palm oil. A simple sample preparation involving alumina as a fat retainer and methanol : acetonitrile (1 : 1) as the extraction solvent was performed prior to the usage of online SPE-LC system. This system consists of two columns, C16for the solid phase extraction (SPE) and C18as the analytical column, and a photo diode array detector. The calibration curves were linear from 5 to 1000 μg L−1, with correlation coefficients above 0.99. The instrumental limit of detection was 3 μg L−1and satisfactory recovery was obtained. A screening on a few samples in the retail market revealed the presence of dibutyl phthalate (DBP) and butylbenzylphthalate (BBP) in the palm oil, with concentration less than 1 mg L−1.

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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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