Abstract
In this study, a highly sensitive and reliable microextraction method, known as in tube ultrasonic and air assisted liquid-liquid microextraction (IT-UAA-LLME), was developed for the preconcentration of some phthalate esters, such as dimethyl phthalate, diethyl phthalate (DEP), di-butyl-phthalate (DBP), bis(2-ethylhexyl) phthalate (BEHP), butyl benzyl phthalate (BBP), and di n-octyl-phthalate (DNOP), prior to their determination using gas chromatography-mass spectrometry (GC-MS). In this technique, the extraction solvent was dispersed into the aqueous sample solution using an ultrasonic bath. The effects of solvent type, aeration time and salt concentration were investigated. After extraction, an organic solvent was injected into the GC-MS instrument for quantification. Under optimum conditions, the enrichment factors ranged from 100 to 330. The calibration curves showed good linearity (r2 > 0.99) and limit of detections were obtained in the range of 0.1-2.1 ng mL-1 in the working concentration ranges. The method was successfully applied for determination of six phthalate esters in real samples with complex matrices with relative standard deviation less than 8%, recovery 88-112% and thus, satisfactory results were obtained.
Highlights
Phthalates or phthalate esters (PEs) are esters of phthalic acid and are mainly used as plasticizers
Air-assisted liquid-liquid microextraction (AALLME) was used for first time for extraction of some phthalate esters, which used a new version of dispersive liquid-liquid microextraction (DLLME) method for extraction and preconcentration of phthalate esters, dimethyl phthalate (DMP), diethyl phthalate (DEP), di-isobutyl phthalate (DIBP), di-n-butyl phthalate (DNBP), and bis(2-ethylhexyl) phthalate (BEHP), from aqueous samples prior to gas chromatography-flame ionization detection (GC-FID).[17]
It is very important to optimize them in order to obtain good recovery, high enrichment factor (EF) and low limit of detection (LOD)
Summary
Phthalates or phthalate esters (PEs) are esters of phthalic acid and are mainly used as plasticizers (substances added to plastics to increase their flexibility, transparency, durability, and longevity). Ultrasonic radiation is a powerful aid, which can accelerate various steps of the analytical process, and ultrasound-assisted emulsification-microextraction (USAEME) has been used as an alternative method for conventional liquid-liquid extraction (LLE).[13,14,15,16] the production of tiny air bubble and good dispersion of extraction solvent in the aqueous phase are important. Air-assisted liquid-liquid microextraction (AALLME) was used for first time for extraction of some phthalate esters, which used a new version of DLLME method for extraction and preconcentration of phthalate esters, dimethyl phthalate (DMP), DEP, di-isobutyl phthalate (DIBP), di-n-butyl phthalate (DNBP), and bis(2-ethylhexyl) phthalate (BEHP), from aqueous samples prior to gas chromatography-flame ionization detection (GC-FID).[17]. The gas chromatograph was fitted with a DB-5 ms capillary column (30 m, 0.25 mm i.d., 0.25 mm film thickness)
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