Residue determination of glyphosate in environmental water samples with high-performance liquid chromatography and UV detection after derivatization with 4-chloro-3,5-dinitrobenzotrifluoride

Qian, Kun; Tang, Tao; Shi, Tianyu; Fang, Wang; Li, Jianqiang; Cao, Yongsong

doi:10.1016/j.aca.2009.01.022

Cited by 87 publications

(62 citation statements)

References 38 publications

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“…15,16 A ausência de grupos cromóforos que absorvem no UV-Vis ou fluoróforos em sua estrutura dificulta a quantificação deste analito, havendo, portanto, a necessidade de aplicação de técnicas de derivatizações (pré-ou pós-coluna), nas determinações cromatográficas. [23][24][25] Em geral, as técnicas de derivatização requerem várias etapas para melhorar a resolução e a seletividade do método.…”

Section: Introductionunclassified

Determinação espectrofotométrica por injeção em fluxo de glifosato em formulações comerciais de herbicidas

Silva¹,

Pezza²,

Pezza³

2012

Quím. Nova

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Recebido em 21/2/11; aceito em 8/6/11; publicado na web em 22/7/11 FLOW-INJECTION SPECTROPHOTOMETRIC DETERMINATION OF GLYPHOSATE IN COMMERCIAL FORMULATIONS OF HERBICIDES. A flow injection spectrophotometric procedure for the determination of glyphosate in commercial formulations of herbicides is proposed. The determination is based on the reaction of glyphosate and p-dimethylaminocinnamaldehyde, in acid medium, yielding a colored compound (l máx = 495 nm). Under optimal conditions, Beer's law is obeyed in a concentration range 40-640 mg mL -1 with a correlation coefficient of 0.9996. The detection limit was 8.60 mg mL -1 for glyphosate. The method was successfully applied for the determination of glyphosate in commercial formulations of herbicides. Recovery of glyphosate from various commercial samples of herbicides range from 91.0 to 110%. Keywords: glyphosate; herbicides; flow injection analysis. INTRODUÇÃOO glifosato [N-(fosfonometil)glicina, C 3 H 8 NO 5 P] é um herbicida (agrotóxico) pós-emergente, pertence ao grupo químico glicina substituída e é tóxico para organismos aquáticos, pouco tóxico para organismos do solo, aves e abelhas, e pouco bioacumulável. 1 Os produtos técnicos à base do ingrediente ativo glifosato, em geral, são classificados na classe III (produto perigoso). 2 É um dos herbicidas mais comumente utilizado no mundo, no controle de plantas daninhas e em diversos tipos de culturas, 3 sendo metabolizado a ácido aminometilfosfônico (AMPA) em plantas e solos através da degradação via sarcosina e glicina. 4 No Brasil constata-se o crescente aumento no consumo de agrotóxicos em razão, principalmente, da expansão da fronteira agrícola e do aumento de terras onde é praticado o plantio direto. Dentre os agrotóxicos consumidos, o glifosato é o ingrediente ativo situado em primeiro lugar no ranking de comercialização no país, representando 76% da comercialização da classe de uso de herbicidas, sendo reportada a comercialização de 71 marcas comerciais de produtos formulados à base de glifosato, por 20 diferentes empresas registrantes. 1 Embora o glifosato não seja considerado um sério contaminante para o homem, os efeitos deste herbicida no meio ambiente ainda não foram completamente elucidados. 5 O glifosato é utilizado nas formulações comerciais usualmente associado com o surfactante polioxietilenoamina (POEA), para o qual nenhum limite específico de exposição ocupacional foi estabelecido. Alguns dos efeitos tóxi-cos das formulações são atribuídos à presença desse ingrediente nas formulações comerciais. 4,6 A forte retenção do glifosato pelo solo, sua alta solubilidade em água e permanência no meio ambiente 7-9 podem favorecer o aumento da concentração deste herbicida na natureza e causar significativo impacto ambiental, 10,11 especialmente em efluentes de fábricas produtoras de glifosato, representando sérios riscos a ambientes agrícolas e aquáticos. 12 Há relatos de diversos métodos para a determinação de glifosato em matrizes diversas, incluindo as técnicas de cromatografia em camada delgada (TLC)...

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Section: Introductionunclassified

Determinação espectrofotométrica por injeção em fluxo de glifosato em formulações comerciais de herbicidas

Silva¹,

Pezza²,

Pezza³

2012

Quím. Nova

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“…Most published methods involve liquid extraction of soil followed by cleanup [20][21][22][23]. There have been few reported methods for determining glyphosate in fatty matrices [21,24,25], and none in rape.…”

Section: Introductionmentioning

confidence: 99%

“…High-performance liquid chromatography with fluorescence detection (HPLC-FLD) or ultraviolet detection (HPLC-UV) [23,26,27] have an excellent track record in its determination. Other techniques include capillary electrophoresis [28,29], ion chromatography with conductivity [30] or fluorescence [31], gas chromatography [32,33], immunoassays [34,35], nuclear magnetic resonance [36], and integrated pulse amperometry [37].…”

Section: Introductionmentioning

confidence: 99%

Liquid chromatographic determination of glyphosate and aminomethylphosphonic acid residues in rapeseed with MS/MS detection or derivatization/fluorescence detection

Kaczyński

Łozowicka

2015

Open Chemistry

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“…Existing analytical methods for the detection of these herbicides in waters and other matrices like soils are mainly based on chromatographic techniques, including liquid chromatography (LC) [7][8][9] and capillary electrophoresis (CE), 10 equipped with different detection devices such as ultraviolet (UV), 11 mass spectrometry (MS), 12,13 and fluorescence detection. [14][15] During the last decade, MS detection with LC separation (LC-MS) has been the technique of choice for the analysis of these herbicides because it provides higher sensitivity and capability to differentiate overlapping peaks with distinct mass-to-charge ratios.…”

Section: Introductionmentioning

confidence: 99%

“…10,15 The analytical challenge posed by these herbicides is that they have neither chromophores nor fluorophores groups, preventing their detection by ultraviolet-visible (UV-vis) absorbance or fluorescence. Because of that, derivatization reactions are needed and the most commonly used are 9-fluorenyl methyl chloro formate (FMOC-Cl), [7][8][9] 4-chloro-3,5-dinitrobenzotrifluoride (CNBF), 11 4-fluoro-7-nitro-2,1,3-benzoxadiazole-(NBD-F), 16 p-toluenesulfonyl chloride (TsCl),17 3,6-dimethoxy-9-phenyl-9H-carbazole-1-sulfonyl chloride (DPCS-Cl), 18 sulfoindocyanine succinimidyl ester (Cy5), 14 FITC and DTAF are both fluorescein-based amino-reactive derivatives, which have relatively high absorptivity and excellent fluorescence quantum yield. What is more attractive is that they have a fluorophore compatible with the LIF detection system (488 or 473 nm).…”

Section: Introductionmentioning

confidence: 99%

Determination of Herbicides and Its Metabolite in Soil and Water Samples by Capillary Electrophoresis-laser Induced Fluorescence Detection Using Microwave-assisted Derivatization

et al. 2014

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Methods were developed to determine glufosinate (GLUF), glyphosate (GLYP) and its metabolite, aminomethylphosphonic acid (AMPA) by capillary electrophoresis-laser induced fluorescence detection using 5-(4,6-dichlorotriazinylamino) fluorescein (DTAF) and fluorescein isothiocyanate (FITC) as the derivatizing reagents. To accelerate the labeling speed, a microwave-assisted derivatization method was adopted. The derivatizing reaction time was reduced to 180 and 150 s for DTAF and FITC, whose reaction time for conventional labeling was 50 min and 5 h, respectively. The optimum separation conditions for derivatives were as follows: a back ground electrolyte (BGE) of 30 mmol L -1 sodium tetraborate containing 15 mmol L -1 brij-35, hydrodynamic injection 15 s and a 10 kV separation voltage. Under these conditions, the LODs (S/N = 3) for DTAF derivatives were 0.32, 0.19 and 0.15 nmol L -1 for GLUF, GLYP, and AMPA, respectively. The LODs (S/N = 3) for FITC derivatives were 2.60, 3.88 and 2.42 nmol L -1 for GLUF, GLYP, and AMPA, respectively. The applicability of the developed method was demonstrated by the detection of the above herbicides and metabolite in water and soil samples.

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Residue determination of glyphosate in environmental water samples with high-performance liquid chromatography and UV detection after derivatization with 4-chloro-3,5-dinitrobenzotrifluoride

Cited by 87 publications

References 38 publications

Determinação espectrofotométrica por injeção em fluxo de glifosato em formulações comerciais de herbicidas

Determinação espectrofotométrica por injeção em fluxo de glifosato em formulações comerciais de herbicidas

Liquid chromatographic determination of glyphosate and aminomethylphosphonic acid residues in rapeseed with MS/MS detection or derivatization/fluorescence detection

Determination of Herbicides and Its Metabolite in Soil and Water Samples by Capillary Electrophoresis-laser Induced Fluorescence Detection Using Microwave-assisted Derivatization

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