scholarly journals AVALIAÇÃO DA PRESENÇA DE PESTICIDAS N-METILCARBAMATOS E SEUS PRODUTOS DE DEGRADAÇÃO NAS ÁGUAS DA REGIÃO DE PARÁ DE MINAS (MG) BRASIL

2001 ◽  
Vol 11 ◽  
Author(s):  
FABRÍCIO VILELA PARREIRA ◽  
EUCLER B. PANIAGO ◽  
CIOMARA RABELO DE CARVALHO ◽  
ROBSON JOSÉ DE CÁSSIA FRANCO AFONSO
Keyword(s):  
Water Samples ◽  
High Performance ◽  
Solid Phase ◽  
Degradation Products ◽  
Phase Extraction ◽  
Method Detection Limit ◽  
Ultraviolet Detector ◽  
Brazilian Legislation ◽  
Relative Standard ◽  
The City

Os pesticidas N-metilcarbamatos e alguns de seus metabólitos são altamente tóxicos para o homem e o meio ambiente. Por esta razão desenvolveu-se método analítico utilizando extração em fase sólida e cromatografia líquida de alta eficiência com detector de ultravioleta (CLAE/UV) para análise destes compostos em amostras de água. O método apresentou índice de recuperação para 10 compostos de 57 a 99%, com desvio padrão relativo (CV) de 5,67 a 7,67% para n=6. A repetitividade do método forneceu CV entre 5,94 a 8,46% para n=6. O limite de detecção do método (MDL) situou-se na faixa de 0,07 a 0,38 µg/L para 10 compostos. Este método foi aplicado na análise de amostras de águas coletadas na cidade de Pará de Minas-MG, Brasil, e também em alguns pontos selecionados nas bacias dos Rios Paciência e Bom Sucesso, situadas no município de Pará de Minas. Os resultados das análises em amostras de água mostraram-se abaixo dos limites estabelecidos pela legislação brasileira. EVALUATION OF THE PRESENCE OF N-METHYLCARBAMATE PESTICIDES AND DEGRADATION PRODUCTS IN WATERS OF PARÁ DE MINAS (MG) REGION IN BRAZIL Abstract The N-methylcarbamate pesticides and some of the their metabolites are highly toxic for men and environment. Then, an analytical method utilizing solid phase extraction and high performance liquid chromatography with ultraviolet detector (SPE/CLAE/UV) to analyze these compounds in water was developed. The accuracy of the method for 10 compounds varied from 57 to 99%, presenting relative standard deviation (RSD) from 5,67 to 7,67% for n=6. The repeatability supplied RSD among 5,94 to 8,46% for n=6. The method detection limit (MDL) is in the ranging of 0,07 to 0,38 µg/L for 10 compounds. This method was utilized in water samples collected in the city of Pará de Minas (MG) and in several points of the rivers Paciência e Bom Sucesso, situated in Pará de Minas (MG), Brazil. The results of the analysis of water samples are bellow of the limits permitted by Brazilian legislation.

scholarly journals Determining the Levels of Four Phenylethanoid Glycosides and Five Triterpene Acids in Liuwei Dihuang Capsule Using Solid Phase Extraction with HPLC-UV

2019 ◽  
Vol 2019 ◽  
pp. 1-9
Author(s):  
Yong Zhang ◽  
Xian-Liang Zou ◽  
Yong-Li Wang ◽  
Lu Gao ◽  
Gui-Xin Chou
Keyword(s):  
Solid Phase Extraction ◽  
High Performance ◽  
Solid Phase ◽  
Phase Extraction ◽  
Phenylethanoid Glycosides ◽  
Triterpene Acids ◽  
Ultraviolet Detector ◽  
Relative Standard ◽  
Removal Of Impurities

In this study, we used quantitative high-performance liquid chromatography equipped with an ultraviolet detector (HPLC-UV) and solid phase extraction (SPE) to determine the levels of four phenylethanoid glycosides and five triterpene acids in Liuwei Dihuang capsules (LDCs). LDCs were methanol-extracted and purified using a 500 mg/6 mL silica-based C18 SPE cartridge. Two elutions were analyzed on a ChromCore C18 column under two HPLC conditions. To improve the pretreatment clean-up, an array of silica- and polymer-based SPE cartridges were compared. Both wash and elution steps were also optimized to achieve the highest removal of impurities. Under optimal chromatographic conditions, good linearity was achieved for all compounds (correlation coefficient of r ≥ 0.999), with a quantification limit ranging from 0.0076 to 0.418 μg/mL. The method had satisfactory efficiency and reproducibility with recovery rates ranging from 91.6 to 99.3% with a relative standard deviation below 1.5%. Taken together, this demonstrated SPE as a suitable extension of HPLC-UV for the determination of phenylethanoid glycosides and triterpene acids in complex LDCs.

Benzoxazine Porous Organic Polymer as an Efficient Solid-Phase Extraction Adsorbent for the Enrichment of Chlorophenols from Water and Honey Samples

2020 ◽  
Author(s):  
Weihua Liu ◽  
Shuangju Song ◽  
Lin Hao ◽  
Chun Wang ◽  
Qiuhua Wu ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Water Samples ◽  
High Performance ◽  
Solid Phase ◽  
Organic Polymer ◽  
Array Detector ◽  
Phase Extraction ◽  
Porous Organic Polymer ◽  
Alternative Approach ◽  
Relative Standard

Abstract Porous organic polymers have gained great research interest in the field of adsorption. A benzoxazine porous organic polymer (BoxPOP) constructed from p-phenylenediamine, 1,3,5-trihydroxybenzene and paraformaldehyde was fabricated and explored as an adsorbent for solid-phase extraction (SPE) of four chlorophenols from water and honey samples. Under the optimized SPE conditions, the response linearity for the analysis of the SPE extract of the chlorophenols by high performance liquid chromatography-diode array detector was observed in the range of 0.2–40.0 ng mL−1 for water samples and 5.0–400.0 ng g−1 for honey samples. The method detection limits of the analytes were 0.06–0.08 ng mL−1 for water samples and 1.5–2.0 ng g−1 for honey samples. The recoveries of the analytes from fortified water and honey samples ranged from 84.8 to 119.0% with the relative standard deviations below 8.4%. The results indicate that the prepared BoxPOP is an effective adsorbent for the chlorophenols. The established method provides an alternative approach for the determination of chlorophenols in real samples.

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 >90% and relative standard deviations ≤16%.

scholarly journals Determination of Patulin in Apple Juice: Comparative Evaluation of Four Analytical Methods

2007 ◽  
Vol 90 (1) ◽  
pp. 162-166 ◽  
Author(s):  
David R Katerere ◽  
Sonja Stockenström ◽  
Gabriele Balducci ◽  
Gordon S Shephard
Keyword(s):  
Comparative Evaluation ◽  
High Performance ◽  
Apple Juice ◽  
Solid Phase ◽  
Phase Extraction ◽  
Low Concentrations ◽  
Relative Standard ◽  
Purification Methods ◽  
Union Directive

Abstract The performance of 4 purification methods for the analysis of patulin in apple juice was evaluated by high-performance liquid chromatography (HPLC). Samples were spiked with patulin at 10, 20, 50, 100, and 150 ppb (ng/mL) and extracted by one of 4 methods (3 solid-phase extraction and one liquidliquid extraction), and then analyzed by HPLCUV under the same isocratic conditions. The methods were validated for recovery, linearity, and precision at high and low concentrations. Recoveries were all >70% for spiking range 10-150 ppb. The relative standard deviation for repeatability was found to meet European Union Directive requirements. In addition, all the methods showed baseline separation from hydroxymethylfurfural.

scholarly journals Magnetic Solid Phase Extraction using Magnetic Mesoporous Silica for Preconcentration of Organophosphorus Pesticides

2019 ◽  
Vol 8 (4) ◽  
pp. 6847-6852
Keyword(s):  
Mesoporous Silica ◽  
Solid Phase Extraction ◽  
Water Samples ◽  
High Performance ◽  
Solid Phase ◽  
Organophosphorus Pesticides ◽  
Magnetic Solid Phase Extraction ◽  
Phase Extraction ◽  
Magnetic Solid ◽  
Mcm 41

The present study describes the synthesis, characterization and application of two mesoporous silica material based coated magnetic nanoparticles namely Fe3O4 -SBA-15 and Fe3O4 -MCM-41 for the simultaneous preconcentration of three selected organophosphorus pesticides (OPPs) namely chlorpyrifos, diazinon and parathion methyl from water samples. The resultant sorbent material was physicochemically and morphologically characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and N2 adsorption analysis. OPPs pesticides extraction efficiency of two sorbents were evaluated through magnetic solid phase extraction (MSPE) using high performance liquid chromatography with ultraviolet detector (HPLC/UV). The main parameters affecting the sorbent efficiency namely extraction time and desorption solvent were optimized. Comparatively, Fe3O4 -SBA-15 achieved excellent percent recovery (97.5%) compared to the Fe3O4 -MCM-41 (87.1%) under optimum condition respectively. The result appealed that the Fe3O4 -SBA-15 composite was efficient sorbent with good capability for the preconcentration of selected OPPs from water samples.AThe present study describes the synthesis, characterization and application of two mesoporous silica material based coated magnetic nanoparticles namely Fe3O4 -SBA-15 and Fe3O4 -MCM-41 for the simultaneous preconcentration of three selected organophosphorus pesticides (OPPs) namely chlorpyrifos, diazinon and parathion methyl from water samples. The resultant sorbent material was physicochemically and morphologically characterized by field emission scanning electron microscopy (FESEM), X-ray diffraction (XRD) and N2 adsorption analysis. OPPs pesticides extraction efficiency of two sorbents were evaluated through magnetic solid phase extraction (MSPE) using high performance liquid chromatography with ultraviolet detector (HPLC/UV). The main parameters affecting the sorbent efficiency namely extraction time and desorption solvent were optimized. Comparatively, Fe3O4 -SBA-15 achieved excellent percent recovery (97.5%) compared to the Fe3O4 -MCM-41 (87.1%) under optimum condition respectively. The result appealed that the Fe3O4 -SBA-15 composite was efficient sorbent with good capability for the preconcentration of selected OPPs from water samples.

scholarly journals Simultaneous Determination of Nitroimidazole Residues in Honey Samples by High-Performance Liquid Chromatography with Ultraviolet Detection

2007 ◽  
Vol 90 (3) ◽  
pp. 872-878 ◽  
Author(s):  
Jinhui Zhou ◽  
Jianzhong Shen ◽  
Xiaofeng Xue ◽  
Jing Zhao ◽  
Yi Li ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Simultaneous Determination ◽  
High Performance ◽  
Solid Phase ◽  
Phase Extraction ◽  
Ultraviolet Detection ◽  
Ultraviolet Detector

Abstract A rapid and sensitive high-performance liquid chromatography (LC) method was developed for the simultaneous determination of metronidazole (MNZ), dimetridazole (DMZ), ronidazole (RNZ), tinidazole (TNZ), and 2-hydroxymethyl-1-methyl-5-nitroimidazole (HMMNI) in honey. After extraction with ethyl acetate and evaporation, the residue containing the nitroimidazoles was dissolved in ethyl acetatehexane and subjected to solid-phase extraction cleanup by amine extraction columns. The effluent was evaporated to dryness, and residues were dissolved and determined by LC with an ultraviolet detector set at 315 nm. The limits of detection were 1.02.0 ng/g for MNZ, DMZ, RNZ, TNZ, and HMMNI in honey. Average recoveries ranged from 71.5101.4% in honey fortified at 10, 20, 50, and 100 ng/g. The method was validated for the analysis of real honey samples.

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