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      Determination of gibberellic acid by sequential injection analysis using a potentiometric detector based on Mn(III)-porphyrin with improved characteristics

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          Abstract

          This work describes the determination of gibberellic acid in growth promoters formulations used in agriculture by sequential injection analysis and potentiometric detection. The potentiometric detectors with improved characteristics used a PVC membrane prepared with Mn(III)tetraphenylporphyrin-Cl as electroactive specie. Different membranes formulated with several ionic additives were compared in order to select the most suitable one concerning slope, response time, reproducibility and selectivity. A membrane containing 6 wt% of manganese tetraphenylporphyrin-Cl [(Mn(TPP)Cl], 27 wt% of PVC, 66 wt% of dibutylphthalate (DBP), as mediator solvent, and 1 wt% of sodium tetraphenylborate, as anionic additive, was chosen for analytical applications. When coupled to a SIA system the tubular electrode presented a linear range between 5×10-4 mol L-1 and 8×10-3 mol L-1, a slope of -64.5 ± 1.6 mV/dec and lower potentiometric selectivity coefficients (log Kpot) than those obtained with the conventional electrodes. Standard deviation of 0.01 and 0.4 (n= 4) and a sampling rate of 30 samples/hour were obtained in the analysis of real samples.

          Translated abstract

          Descreve-se a determinação de ácido giberélico em promotores de crescimento usados na agricultura, por análise de injecção sequencial e detecção potentiométrica. Os detectores potentiométricos com características melhoradas usam uma membrana de PVC preparada com Mn(III)tetrafenilporfirina-Cl ([(Mn(TPP)Cl]). Formularam-se diferentes membranas comparando-se aditivos iónicos com o objectivo de se seleccionar as unidades com as melhores características de declive, tempo de resposta, reprodutibilidade e selectividade. Para fins analíticos foi seleccionada uma membrana com 6% de [(Mn(TPP)Cl], 27% de PVC, 66% de dibutilftalato (DBP), como solvente mediador, e 1% de tetrafenilborato de sódio, como aditivo aniónico. Quando inserido num sistema SIA o eléctrodo tubular apresentava um intervalo de linearidade de 5×10-4 mol L-1 a 8×10-3 mol L-1, declive de -64,5 ± 1,6 mV/dec e melhores coeficientes de selectividade potenciométrica (log Kpot) do que os obtidos com eléctrodos convencionais. Na análise de amostras comercializadas em Portugal obtiveram-se desvios padrão de 0,01 e 0,4 (n= 4) e um ritmo de amostragem de 30 amostras/hora.

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          Homochiral Porous Organic Cage with High Selectivity for the Separation of Racemates in Gas Chromatography.

          Porous organic molecular cages as a new type of porous materials have attracted a tremendous attention for their potential applications in recent years. Here we report the use of a homochiral porous organic cage (POC) (CC3-R) diluted with a polysiloxane (OV-1701) as a stationary phase for high-resolution gas chromatography (GC) with excellent enantioselectivity. A large number of optical isomers have been resolved without derivatization, including chiral alcohols, diols, amines, alcohol amines, esters, ketones, ethers, halohydrocarbons, organic acids, amino acid methyl esters, and sulfoxides. Compared with commercial β-DEX 120 and Chirasil-L-Val columns, the CC3-R coated capillary column offered more preeminent enantioselectivity. In addition, CC3-R also exhibits good selectivity for the separation of isomers, linear alkanes, alcohols, and aromatic hydrocarbons. The excellent resolution ability, repeatability, and thermal stability make CC3-R a promising candidate as a novel stationary phase for GC. The study described herein first proves useful commercially. This work also indicates that porous organic molecular materials will become more attractive in separation science.
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            Assessment of a 1H high-resolution magic angle spinning NMR spectroscopy procedure for free sugars quantification in intact plant tissue.

            In most plants, sucrose is the primary product of photosynthesis, the transport form of assimilated carbon, and also one of the main factors determining sweetness in fresh fruits. Traditional methods for sugar quantification (mainly sucrose, glucose and fructose) require obtaining crude plant extracts, which sometimes involve substantial sample manipulation, making the process time-consuming and increasing the risk of sample degradation. Here, we describe and validate a fast method to determine sugar content in intact plant tissue by using high-resolution magic angle spinning nuclear magnetic resonance spectroscopy (HR-MAS NMR). The HR-MAS NMR method was used for quantifying sucrose, glucose and fructose in mesocarp tissues from melon fruits (Cucumis melo var. reticulatus and Cucumis melo var. cantalupensis). The resulting sugar content varied among individual melons, ranging from 1.4 to 7.3 g of sucrose, 0.4-2.5 g of glucose; and 0.73-2.83 g of fructose (values per 100 g fw). These values were in agreement with those described in the literature for melon fruit tissue, and no significant differences were found when comparing them with those obtained using the traditional, enzymatic procedure, on melon tissue extracts. The HR-MAS NMR method offers a fast (usually <30 min) and sensitive method for sugar quantification in intact plant tissues, it requires a small amount of tissue (typically 50 mg fw) and avoids the interferences and risks associated with obtaining plant extracts. Furthermore, this method might also allow the quantification of additional metabolites detectable in the plant tissue NMR spectrum.
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              Anal. Chim. Acta

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                Author and article information

                Contributors
                Role: ND
                Role: ND
                Role: ND
                Role: ND
                Role: ND
                Journal
                jbchs
                Journal of the Brazilian Chemical Society
                J. Braz. Chem. Soc.
                Sociedade Brasileira de Química (São Paulo )
                1678-4790
                October 2004
                : 15
                : 5
                : 701-707
                Affiliations
                [1 ] Faculty of Pharmacy Portugal
                [2 ] ISCS Portugal
                [3 ] Universidade de São Paulo Brazil
                Article
                S0103-50532004000500015
                10.1590/S0103-50532004000500015
                1370c3ee-94c0-4ea2-8f49-d50e9316aea5

                http://creativecommons.org/licenses/by/4.0/

                History
                Product

                SciELO Brazil

                Self URI (journal page): http://www.scielo.br/scielo.php?script=sci_serial&pid=0103-5053&lng=en
                Categories
                CHEMISTRY, MULTIDISCIPLINARY

                General chemistry
                gibberellic acid,ion selective tubular electrode,SIA,metalloporphyrins,agricultural growth promoters

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