Solvent-vapor-assisted liquid-liquid microextraction: A novel method for the determination of phthalate esters in aqueous samples using GC-MS

Abstract

A novel liquid-liquid microextraction method, namely, solvent-vapor-assisted liquid-liquid microextraction for the determination of dimethyl phthalate, diethyl phthalate, dibutyl phthalate and bis(2-ethylhexyl) phthalate in the aqueous samples using gas chromatography with mass spectrometry was developed. In the proposed method, extracting solvent was heated, and solvent vapor as the extracting phase was injected into the sample solution. As a result of the low temperature of the sample solution and higher density of the extracting phase than the aqueous medium, solvent vapor was condensed and an organic-phase drop formed in the bottom of sample tube. Because of the gas status of the extracting solvent, the surface area between the extracting solvent and the aqueous sample was remarkably high. Under the optimized conditions, tetrachloride carbon was used as an extracting solvent. The method shows high coefficient of determination (R ) values in the range of 0.5-200 and 1.0-200 ng/mL for the target analytes. Enrichment factors and limits of detection for the studied phthalates are obtained in the ranges of 2800-3000 and 0.15-0.3 ng/mL, respectively. Recoveries and relative standard deviations were in the range of 80.0-100.0 and 2.2-7.8%, respectively. The proposed method successfully used for analysis of several aqueous samples.

Bisphenol and Phthalate Migration Test from Mexican Meat Packaging Using HPLC-DAD Technique

“…6 and S7 presents a nonspiked E-1 sample chromatogram and spiked E-1 Sample chromatogram, respectively, in supplementary materials) and guaranteed the reliability of the optimized method [31]. About the DEP and DBP percentage recoveries, their results were in accord with the LLME-GC-MS method (80-100%) proposed by Mohebbi et al [25].…”

“…e sensitivity of the proposed method was lower than that obtained in different studies [10,22,23,25] since they use detectors with greater sensitivity and preconcentration stages of the sample before the detection of analytes. For example, Moreira et al (2014) used solid-phase microextraction (SPME), which is well-known for allowing analyte preconcentration and sample purification.…”

“…Analytical schemes have been reported in the literature. e detection of very low concentrations can be carried out by high-performance liquid chromatography (HPLC) with diode array detection (DAD) [11,20,21] high performance liquid chromatography coupled to tandem mass spectrometry (HPLC-MS/MS) [10], cold fiber solid-phase microextraction (CF-SPME-GC-MS) [22], high performance liquid chromatography, ultraviolet detection (HPLC-UV) [23,24], and liquid-liquid microextraction chromatography with mass spectrometry (LLME-GC-MS) [25][26][27].…”

Simultaneous determination of paracetamol and caffeine in aqueous samples by ultrasound‐assisted emulsification microextraction coupled with high‐performance liquid chromatography

“…On the other hand, it has several drawbacks such as use of large volumes of organic solvents which lead to environmental pollution, small enrichment factor, problems with sample handling due to large volume of sample and time consuming. In recent decades, the introduction of effective liquid-liquid microextraction (LLME) methods has reduced the abovementioned drawbacks [13][14][15][16][17][18][19][20][21][22][23][24][25][26][27].…”