Liquid chromatographic determination of linear alkylbenzenesulfonates in aqueous environmental samples

Corcia, Antonio Di; Marchetti, M. C.; Samperi, Roberto; Marcomini, Antonio

doi:10.1021/ac00011a023

Cited by 82 publications

(41 citation statements)

References 19 publications

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“…[4][5][6] However, some derivatization steps to convert LAS into a volatile compound 7,8 are unavoidable for GC procedures, because LASs are not volatile enough to permit direct measurement by GC. LC has widely been applied to the determination of LAS in various environmental samples without any derivatization using ultraviolet (UV), 9-11 fluorescence (FL), [12][13][14][15][16] and MS [17][18][19] detection. Nakae et al 12,13 obtained an excellent separation of many LAS components (homologues and isomers) by reversed-phase chromatography with FL detection.…”

Section: Introductionmentioning

confidence: 99%

Characterization and Determination of Linear Alkylbenzenesulfonates in Environmental Water Samples by High-Performance Liquid Chromatography with a Hydrophilic Polymer Column and Electrospray Ionization Mass Spectrometric Detection

2004

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A liquid chromatography-mass spectrometry (LC/MS) method was developed for the separation and determination of linear alkylbenzenesulfonates (C10 -C14 LAS) in environmental water samples using a hydrophilic polymer column . This method involves a solid-phase extraction of the LAS samples with a Sep-Pak PS-2 cartridge. The LAS components were separated on the column with a mobile phase of 29% (w/v) acetonitrile-water containing 0.8 mM di-n-butylammonium acetate and 0.2 M acetic acid, and were detected by mass spectrometry with electrospray ionization. Detection limits of the developed method based on selected ion monitoring (SIM) technique for the C10 -C14 LAS standards were 13 -47 ng L -1 . The concentrations of the C10 -C14 LAS in the environmental water samples ranged between 5 -317 µg L -1 for a river water sample and 0.4 -6.4 µg L -1 for a seawater sample. Linear relationships between the logarithms of retention factors and the alkyl chain lengths for each phenyl positional isomer of LAS could successfully be used for the identification of the isomer peaks.

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Section: Introductionmentioning

confidence: 99%

Characterization and Determination of Linear Alkylbenzenesulfonates in Environmental Water Samples by High-Performance Liquid Chromatography with a Hydrophilic Polymer Column and Electrospray Ionization Mass Spectrometric Detection

2004

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“…The use of a gradient system results in a better separation of the individual LAS homologues. 33 Excellent separations of the peaks of homologues of LAS were obtained from the usage of the C-8 column as the stationary phase and the LAS homologues were separated with high resolution, with retention times of 14, 17, 20 and 23 minutes for peaks 1, 2, 3 and 4, respectively and all the isomers of each LAS homologue co-elutes into a single peak, 16 facilitating the interpretation of the chromatogram. These obtained results were the opposite of those obtained with the C-18 column, 15,[33][34][35] where the LAS homologues cannot be separated as different peaks.…”

Section: Effect Of the Column And The Mobile Phase On The Las Separationmentioning

confidence: 99%

“…15 This method, however, can be applied only to relatively clean aqueous samples that have quite high contents of LAS. 16 The Reversed-phase HPLC must be considered the routine method for LAS analysis. 17 Liquid chromatography procedures for separation and determination of LAS surfactants usually employ C-8 or C-18 columns and mobile phases containing organic substances and water.…”

Section: Introductionmentioning

confidence: 99%

“…This mobile phase commonly contains an electrolyte, [18][19][20] anion exchangers, 21 or reversed stationary phases in combination with mobile phases containing ionic interaction reagents such as quaternary ammonium salts. 16 The reversed-phase HPLC method provides the separation of LAS mixture and may use various chromatographic detectors, as spectrometry ultraviolet (UV), 22 fluorescence 4,23,24 and mass spectrometry (MS). 25,26 Most HPLC methods with UV detector require the mobile phase to contain either sodium perchlorate 25 or additive, such as triethylamine and acetic acid.…”

Section: Introductionmentioning

confidence: 99%

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Development of a method by HPLC to determine LAS and its application in anaerobic reactors

Duarte¹,

Oliveira²,

Buzzini³

et al. 2006

J. Braz. Chem. Soc.

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Este trabalho descreve o desenvolvimento e a validação de um método que usa cromatografia líquida de alta eficiência para determinação de Alquilbenzeno Linear Sulfonado (LAS) em amostras de águas provenientes de reatores anaeróbios. O padrão de LAS aplicado foi ácido dodecilbenzeno sulfônico-sal sódico, que apresentou 4 picos principais no cromatograma, relacionados aos diferentes homólogos da cadeia alquílica linear. Diferentes condições cromatográficas foram testadas, tais como, fases estacionárias C-18, C-12 e C-8; detectores de ultravioleta e de fluorescência, composição da fase móvel e tempo de programação do gradiente de eluição. A melhor condição cromatográfica obtida foi com a coluna C-8, fase móvel: metanol/ perclorato de sódio 0,075 mol L -1 e detector de fluorescência. A validação deste método foi feita através das curvas de calibração de LAS, usando água e substrato sintético como solventes. O método foi validado com o objetivo de demonstrar sua precisão, linearidade, limite de detecção para cada homólogo e a sua precisão instrumental.This work describes the development and validation of a method using High Performance Liquid Chromatography (HPLC) for Linear Alkylbenzene Sulfonate (LAS) determination in sample of wastewater from anaerobic reactors. The applied LAS standard was the dodecylbenzene sulfonic acid-sodium salt, which presents four main peaks in the chromatogram, related to different homologous of the linear alkyl chain. Different chromatographic conditions were tested with C-18, C-12 and C-8 as stationary phases, ultraviolet and fluorescence detectors, mobile phase (MP) compositions and programming time of elution gradient. The best chromatographic condition was obtained with the C-8 column, MP: methanol and of sodium perchlorate (0.075 mol L -1 ). The validation of this method was made with the calibration of LAS curves using water and synthetic substrate as solvents. The method was validated in order to demonstrate its precision, linearity, limit of detection of each homolog and its instrumental precision.

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“…Ion-exchange HPLC is useful in identifying surfactant classes but inefficient in separating LAS homologues and isomers [18,24]. Isocratic [13,17] and gradient [14-16, 19-22, 25, 26, 33] procedures with spectrophotometric [15,16,20,21], fluorimetric [13,16,17,19,20,22,25,33] and mass spectrometric [14,[26][27][28]33] detection have been described in reversed-phase HPLC. For instance, the LAS homologues can be resolved using a C 8 column and a mobile phase containing sodium perchlorate in methanol/water [17], while a C 18 column and a mobile phase containing sodium perchlorate in acetonitrile/water may be used to separate the isomers [12,15,[19][20][21].…”

Section: Introductionmentioning

confidence: 99%

Separation of homologues and isomers of linear alkylbenzenesulfonates by capillary electrophoresis with sodium dodecyl sulfate, carboxylic acids and bile salts

2003

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The ability of several anionic compounds, including carboxylic and dicarboxylic acids, sodium dodecyl sulfate (SDS), and sodium deoxycholate (SDC) and other bile salts, to separate the C(10)-C(13) homologues and the corresponding 20 positional isomers of linear alkylbenzenesulfonates (LAS) by capillary electrophoresis was studied. Up to 19 peaks and a shoulder were observed with a background electrolyte (BGE) containing 10 mM phosphate (pH 6.8), 30% acetonitrile and 40 mM SDS, and 18 peaks were obtained with a BGE containing 10 mM borate (pH 9), 40% ethanol and 40 mM palmitic acid (PA). Resolution increased with the alkyl chain length of the carboxylic acid. Dicarboxylic acids with a short alkyl chain, as azelaic acid, were useful to separate the homologues without distinguishing between the isomers. Up to 16 peaks and a shoulder were distinguished with SDC. Resolution decreased with the other bile salts. The 6-C(11)/5-C(11) isomer pair was better resolved with SDC than with SDS, and the 2-C(12) isomer was isolated using both PA and SDC, but not with SDS. Only the 7-C(13)/6-C(13) pair could not be resolved with any of the discriminating agents used.

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Liquid chromatographic determination of linear alkylbenzenesulfonates in aqueous environmental samples

Abstract: not

Cited by 82 publications

References 19 publications

Characterization and Determination of Linear Alkylbenzenesulfonates in Environmental Water Samples by High-Performance Liquid Chromatography with a Hydrophilic Polymer Column and Electrospray Ionization Mass Spectrometric Detection

Characterization and Determination of Linear Alkylbenzenesulfonates in Environmental Water Samples by High-Performance Liquid Chromatography with a Hydrophilic Polymer Column and Electrospray Ionization Mass Spectrometric Detection

Development of a method by HPLC to determine LAS and its application in anaerobic reactors

Separation of homologues and isomers of linear alkylbenzenesulfonates by capillary electrophoresis with sodium dodecyl sulfate, carboxylic acids and bile salts

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