Rapid determination of sixteen sulfonylurea herbicides in surface water by solid phase extraction cleanup and ultra-high-pressure liquid chromatography coupled with tandem mass spectrometry

Yan, Cuimin; Zhang, Beibei; Liu, Wenyuan; Feng, Feng; Zhao, Yuqing; Du, Hui

doi:10.1016/j.jchromb.2011.09.028

Cited by 43 publications

(26 citation statements)

References 20 publications

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“…Esta etapa visa remover seletivamente resíduos de agrotóxicos destas amostras e pré-concentrá-los. 12 As principais técnicas existentes são a extração em fase sólida, [13][14][15] microextração em fase sólida, [16][17][18][19] microextração líquido-líquido [20][21][22][23] e microextração em gota única. 24 Apesar do elevado número de técnicas existentes, a extração líquido-líquido com partição em baixa temperatura (ELL-PBT) tem se apresentado como uma alternativa para extração de agrotóxicos em diversas matrizes.…”

Section: Introductionunclassified

Análise de agrotóxicos em água usando extração líquido-líquido com partição em baixa temperatura por cromatografia líquida de alta eficiência

Silvério¹,

Silva²,

Aguiar³

et al. 2012

Quím. Nova

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Recebido em 22/1/12; aceito em 6/7/12; publicado na web em 31/8/12 ANALYSIS OF PESTICIDES IN WATER USING LIQUID-LIQUID EXTRACTION WITH PARTITION AT LOW TEMPERATURE AND HIGH PERFORMANCE LIQUID CHROMATOGRAPHY. This study optimized and validated the liquid-liquid extraction technique with partition at low temperature (LLE-PLT) for identification and quantification of four pesticides (chlorpyrifos, λ-cyhalothrin, permethrin, bifenthrin) in water samples. Analyses were performed by HPLC-UV. The technique was efficient for pesticide recovery with extraction exceeding 86%. Chromatographic response was linear for the four compounds in the 10-45 µg L -1 range, with correlation coefficients greater than 0.99. Limits of detection and quantitation were less than 3.5 µg L -1 and equal to 10 µg L -1 , respectively. The proposed method was applied to 29 water samples from the Jaíba Project in northern Minas Gerais.Keywords: LLE-LTP; pesticides; HPLC-UV. INTRODUÇÃOO Projeto Jaíba é um amplo projeto de irrigação de grande importância para todo o Norte de Minas.1 A água utilizada para irrigação é coletada em canais próximos às próprias plantações (Figura 1S, material suplementar), apresentando elevado risco de contaminação devido a sua localização geográfica, fenômenos de lixiviação 2,3 e aplicações de agrotóxicos por via aérea. 4 Os agrotóxicos são largamente empregados para minimizar perdas na produtividade, atribuídas ao ataque de pragas. 5,6 A aplicação de agrotóxicos pode gerar resíduos no ar, solo e na água, expondo indiretamente o ser humano.7 Por isso, as agências reguladoras estabelecem limites máximos de resíduo permitido (LMR) em diversas matrizes. 8,9 Esses valores de LMR são estabelecidos levando em consideração vários fatores, dentre eles a toxicidade do composto para seres humanos e o limite de quantificação dos métodos instrumentais de análises. Devido à exigência da legislação e à toxicidade destas substâncias, o consumo desta água ou sua reutilização na agricultura pode resultar em riscos à saúde pública.A região do Projeto Jaíba se destacou nos últimos anos na produção de banana prata, limão tahiti e manga.10 Nestas culturas, clorpirifós, λ-cialotrina, permetrina e bifentrina representam agrotóxicos comuns para o controle de pragas.9 Embora destes quatro agrotóxicos apenas a permetrina seja regulamentada pela Portaria 518 de 2004 em amostras de água, 11 o uso constante dessas substâncias torna a análise e o monitoramento fundamentais para preservar a saúde humana e o meio ambiente.O primeiro passo para análise e monitoramento destas substâncias em água envolve o desenvolvimento da técnica de extração. Esta etapa visa remover seletivamente resíduos de agrotóxicos destas amostras e pré-concentrá-los. 12 As principais técnicas existentes são a extração em fase sólida, 13-15 microextração em fase sólida, 16-19 microextração líquido-líquido 20-23 e microextração em gota única. 24Apesar do elevado número de técnicas existentes, a extração líquido-líquido com partição em baixa temperatura (ELL-PBT) tem se apresentado...

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Section: Introductionunclassified

Análise de agrotóxicos em água usando extração líquido-líquido com partição em baixa temperatura por cromatografia líquida de alta eficiência

Silvério¹,

Silva²,

Aguiar³

et al. 2012

Quím. Nova

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“…As shown in Table S2, a pretreatment time of less than 15 min is significantly shorter than conventional SPE (2-7 h) [2,5,8]. In comparison with reported MSPE-based methods [13,30], our method presents lower LODs for more SUs.…”

Section: Methods Performance Comparisonmentioning

confidence: 82%

“…The most common analytical methods for SUs are high-performance liquid chromatography coupled with an ultraviolet or diode-array detector (HPLC-UV/DAD) [2][3][4][5][6] and mass spectrometry (HPLC-MS) [7,8]. However, for low concentration of SUs in water, UV detectors cannot provide high sensitivity without enrichment prior to analysis.…”

Section: Introductionmentioning

confidence: 99%

“…Therefore, pretreatment techniques are imperative for the enrichment and cleanup of SUs in environmental samples in order to achieve the ideal sensitivity and effectively eliminate contaminants from complex matrices. Currently reported pretreatment techniques for SUs in environmental water samples mainly include solid-phase extraction (SPE) [2,5,7,8], dispersive liquid-liquid microextraction [4], stir-bar sorptive extraction [9], and salting-out assisted liquid-liquid extraction [10]. SPE, due to its high recovery, short extraction time, high enrichment factor, low consumption of organic solvents, and ease of automation and operation, has been widely used to concentrate organic compounds in water samples.…”

Section: Introductionmentioning

confidence: 99%

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Determination of six sulfonylurea herbicides in environmental water samples by magnetic solid-phase extraction using multi-walled carbon nanotubes as adsorbents coupled with high-performance liquid chromatography

Jiang

et al. 2016

Journal of Chromatography A

105

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a b s t r a c tMagnetic solid-phase extraction (MSPE) using magnetic multi-walled carbon nanotubes (mag-MWCNTs) as adsorbents, coupled with high-performance liquid chromatography-diode-array detector (HPLC-DAD), was developed for the simultaneous separation and determination of six types of sulfonylurea herbicides (SUs) in environmental water samples. Several variables affecting MSPE efficiency were systematically investigated, including the type and volume of desorption solvent, sample solution pH, salt concentration, amount of mag-MWCNTs, and extraction and desorption time. Response surface was employed to assist in the MSPE optimization. Under optimized conditions, excellent linearity was achieved in the range of 0.05-5.0 g/L for all six SUs, with coefficients of correlation r > 0.9994, and preconcentration factors ranging from 178 to 210. Limits of detection and quantification were 0.01-0.04 g/L and 0.03-0.13 g/L, respectively. The intra-day and inter-day precision (relative standard deviations, n = 6, %) at three spiked levels were 2.0-11.0% and 2.1-12.9% in terms of peak area, respectively. The method recoveries at three fortified concentrations were obtained within 76.7-106.9% for reservoir water samples and 78.2-105.4% for tap water samples. The developed MSPE-HPLC method demonstrated high sensitivity, repeatability, simplicity, rapidity, and excellent practical applicability.

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“…Chromatography conditions were also evaluated. Regarding the acidic properties of G004, mobile phase with the use of different concentrations of acetic acid was compared to test their effects on MS peak intensity [28,29], and peak efficiencies were improved when acetonitrile instead of methanol was used. Finally, an elution system (acetonitrile-0.05% acetic acid containing 5 mM ammonium acetate) as previously described was chosen.…”

Section: Troubleshooting Of the Metabolite Interferencementioning

confidence: 99%

Interference by metabolites and the corresponding troubleshooting during the LC–MS/MS bioanalysis of G004, a bromine-containing hypoglycemic agent

Ding

et al. 2012

Journal of Chromatography B

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Rapid determination of sixteen sulfonylurea herbicides in surface water by solid phase extraction cleanup and ultra-high-pressure liquid chromatography coupled with tandem mass spectrometry

Cited by 43 publications

References 20 publications

Análise de agrotóxicos em água usando extração líquido-líquido com partição em baixa temperatura por cromatografia líquida de alta eficiência

Análise de agrotóxicos em água usando extração líquido-líquido com partição em baixa temperatura por cromatografia líquida de alta eficiência

Determination of six sulfonylurea herbicides in environmental water samples by magnetic solid-phase extraction using multi-walled carbon nanotubes as adsorbents coupled with high-performance liquid chromatography

Interference by metabolites and the corresponding troubleshooting during the LC–MS/MS bioanalysis of G004, a bromine-containing hypoglycemic agent

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