Extraction and Isolation of Linear Alkylbenzenesulfonate and Its Sulfophenylcarboxylic Acid Metabolites from Fish Samples

Abstract

Linear alkylbenzenesulfonate (LAS) is the most widely used synthetic surfactant. In fish, assessment of the environmental risk and investigation of the biotransformation behavior of LAS require compound-specific methods for extraction and isolation of LAS and its biotransformation products, sulfophenylcarboxylic acids (SPC). Matrix solid-phase dispersion (MSPD) extraction with subsequent ion-pair liquid-liquid (IP-LL) partitioning of the extract was a time-efficient sample preparation method for analysis of LAS. The recovery of parent LAS from spiked fish exceeded 70%, and the limit of quantitation ranged around 0.2 mg.kg-1 corresponding to 0.6 mumol.kg-1. In a simultaneous determination of LAS and SPC in fish, the analytes were MSPD extracted in different fractions. The target compounds were separated from the sample matrix by protein precipitation and subsequent isolation of (a) SPC by graphitized carbon black solid-phase extraction of the supernatant and (b) parent LAS by IP-LL partitioning of the pellet obtained after protein precipitation. The recoveries of the model compounds C12-2-LAS and C4-3-SPC were 84 +/- 6 and 65 +/- 11%, respectively. The use of C3-3-SPC as an internal standard corrected for the loss of the biotransformation product during sample workup. The suitability of both methods was demonstrated by analyzing fish containing LAS and SPC incurred during aqueous exposure.

Analitical Method Validation of Anionic Surfactant Sodium Dodecyl Benzene Sulfonate (Sdbs) in Catfish by Uv-Vis Spectrophotometry Using Acridine Orange

“…Penelitian penentuan konsentrasi surfaktan pada tubuh makhluk hidup dapat dilakukan dengan HPLC dan spektrofotometer (Tolls et al 1999;Saez et al 2000;Datta et al 2002;Purba, 2014), namun metode yang dipergunakan membutuhkan bahan dengan toksisitas tinggi dan kurang ramah lingkungan. Penggunaan HPLC dalam analisis surfaktan menghasilkan sensitivitas yang baik akan tetapi proses preparasi sampel yang lebih lama dan biaya operasional yang mahal serta ketersediaan alat yang terbatas.…”

Analysis of Surfactants in Environmental Samples by Chromatographic Techniques

“…In the case of surfactants, this extraction protocol has been mainly applied to fish samples [99], where aliquots are taken and mixed with octadecyl silica in a column, in order to isolate LAS and SPCs, as well as non-ionic surfactants. Afterwards, strong non-polar solvents (e.g., hexane) and methanol are used to remove fats in a first clean-up stage and to extract surfactants after another elution, respectively.…”

Forensic Toxicological Determination of Surfactant by Liquid Chromatography/Electrospray lonization Mass Spectrometry and Liquid Chromatography/Electrospray lonization Tandem Mass Spectrometry.

“…Surfactants have often been extracted by ODScartridge, 3,4) carbon cartridge, 5) XAD-16, 6) or liquidliquid extraction. 4) We examined the sample preparation of low-concentration surfactant aqueous solution using 1) extraction with the weak anion-exchange cartridge Bond Elut ® PSA; 2) extraction with the weak cation-exchange cartridge Bond Elut ® CBA; 3) liquid-liquid extraction with tertbuthylmethylether; and 4) concentration in a water bath.…”

“…4) We examined the sample preparation of low-concentration surfactant aqueous solution using 1) extraction with the weak anion-exchange cartridge Bond Elut ® PSA; 2) extraction with the weak cation-exchange cartridge Bond Elut ® CBA; 3) liquid-liquid extraction with tertbuthylmethylether; and 4) concentration in a water bath. As samples, we selected anionic surfactants LAS and AES, cationic surfactant BZ, and nonionic surfactant AE in aqueous solutions of 20 ppm.…”

“…The determination of surfactants has so far been performed using the color test with ion-association reagents, 1) high-performance liquid chromatography (HPLC), [2][3][4] etc. As the information acquired with these conventional analytical methods is very limited, their complete structures, molecular mass, or degree of polymerization of ethyleneoxide (EO) has been difficult to obtain.…”