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

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.

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

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
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.

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

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
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.

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

2019 ◽  
Vol 7 (2) ◽  
pp. 245-253 ◽  
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.

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

PLoS ONE ◽  
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.

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

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.

scholarly journals Simultaneous Determination of 23 Mycotoxins in Broiler Tissues by Solid Phase Extraction UHPLC-Q/Orbitrap High Resolution Mass Spectrometry

Separations ◽  
2021 ◽  
Vol 8 (12) ◽  
pp. 236
Author(s):  
Youyou Yang ◽  
Zhuolin He ◽  
Lei Mu ◽  
Yunfeng Xie ◽  
Liang Wang
Keyword(s):  
Mass Spectrometry ◽  
Solid Phase Extraction ◽  
Simultaneous Determination ◽  
Solid Phase ◽  
Harmful Effect ◽  
Phase Extraction ◽  
External Standard Method ◽  
Relative Standard ◽  
Limit Of Quantitation

Mycotoxins are a type of toxins harmful for not only animal but also human health. Cooccurrence of multi-mycotoxins could occur for food infected by several molds, producing multi-mycotoxins. It is necessary to develop corresponding determination methods, among which current mass spectrometry (MS) dominates. Currently, the accurate identification and quantitation of mycotoxins in complex matrices by MS with low resolution is still a challenge since false-positive results are typically obtained. Here, a method for the simultaneous determination of 23 mycotoxins in broiler tissues using ultra-high performance liquid chromatography-quadrupole/orbitrap HRMS was established. After the extraction by acetonitrile-water-formic acid (80:18:2, v/v/v), the purification by multifunctional purification solid phase extraction cartridges and the chromatographic separation on a C18 column, representative mycotoxins were determined by HRMS in full scan/data-dependent MS/MS acquisition mode. The quantitation was based on the external standard method. An MS/MS database of 23 mycotoxins was established to achieve qualitative screening and simultaneous quantification. Mycotoxins had a good linear relationship within a certain concentration range with correlation coefficients (r2) larger than 0.991 as well as the limit of quantitation of 1.80–300 μg/kg. The average recoveries at three different levels of low, medium and high fortification were 61–111% with relative standard deviations less than 13.5%. The method was fast, accurate, and suitable for the precise qualification of multiple mycotoxins in broiler tissues. 15 μg/kg zearalenone (ZEN) was detected in one liver sample among 30 samples from markets including chicken breast meat, liver, and gizzards. The result illustrated that the pollution of ZEN should not be neglected considering its harmful effect on the target organ of liver.

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

2007 ◽  
Vol 90 (2) ◽  
pp. 568-574 ◽  
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.

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

2002 ◽  
Vol 85 (2) ◽  
pp. 375-383 ◽  
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%.

Quantitation of 1α,25-dihydroxyvitamin D by LC-MS/MS using solid-phase extraction and fixed-charge derivitization in comparison to immunoextraction

2015 ◽  
Vol 53 (9) ◽  
Author(s):  
Nancy Chan ◽  
Erin J. Kaleta
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Fixed Charge ◽  
Reference Laboratory ◽  
Phase Extraction ◽  
Dihydroxyvitamin D ◽  
Limit Of Quantitation ◽  
Attractive Option ◽  
Assay Precision

AbstractThe objective of this study was to present analysis of 1α,25-dihydroxyvitamin D (DHVD) by solid-phase extraction (SPE) using fixed-charge derivitization extraction to enhance ionization for liquid chromatography coupled to tandem mass spectrometry (LC-MS/MS) in comparison to traditional immunoextraction (IE) techniques.Full analytical validation of both a SPE and IE LC-MS/MS assay was performed, and included accuracy, intra- and inter-assay precision, limit of detection and limit of quantitation. Performance of these two assays was compared with reference laboratory IE LC-MS/MS testing.This SPE LC-MS/MS assay demonstrated similar performance to the IE LC-MS/MS assay validated simultaneously. Intra-assay precision for low (12 pg/mL), medium (25 pg/mL) and high (60 pg/mL) control samples was 7.2%, 13.7% and 11.3% for DHVD2, respectively, and 9.1%, 5.9% and 8.9% for DHVD3. The inter-assay precision was 11.6%, 10.3% and 3.9% for DHVD2 and 10.6%, 7.0% and 5.6% for DHVD3. The limit of detection was 1.9 and 2.7 pg/mL for DHVD2 and DHVD3, and limit of quantitation was 4 pg/mL for both DHVD2 and DHVD3. Comparison to a reference LC-MS/MS assay showed excellent correlation (slope 0.936, RThe study demonstrated comparability of the SPE-LC-MS/MS assay for analysis of DHVD and offers an attractive option for assessment of vitamin D status as an alternative to traditional IE techniques.

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