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  • Determination of phthalate esters in vegetable oils using direct immersion solid-phase microextraction and fast gas chromatography coupled with triple quadrupole mass spectrometry.

Determination of phthalate esters in vegetable oils using direct immersion solid-phase microextraction and fast gas chromatography coupled with triple quadrupole mass spectrometry.

Analytica chimica acta (2015-09-01)
Laura Barp, Giorgia Purcaro, Flavio A Franchina, Mariosimone Zoccali, Danilo Sciarrone, Peter Q Tranchida, Luigi Mondello
ABSTRACT

Phthalates are a group of synthetic compounds mainly used as plasticizers, which have been classified as endocrine-disrupting chemicals and potential human-cancer causing agents. They can be found in high amounts in foods, deriving mainly from plastic packaging. The analytical determination of these compounds is very challenging since they are ubiquitous. Therefore, minimization of sample manipulation is highly desirable. The present work exploited the application of a solid-phase microextraction method for the analysis of phthalates in vegetable oil. A preliminary comparison between a polydimethylsiloxane (PDMS) and a Carbopack Z/PDMS fiber was carried out both in the headspace and direct immersion extraction modes. Before immersing the fiber, a rapid liquid-liquid extraction was performed using acetonitrile to remove the bulk of triglycerides. PDMS in the direct immersion mode showed the best performance. The method was fully validated obtaining a good linearity with a coefficient of correlation of over 0.9960 for all compounds, repeatability and accuracy values generally better than 10%, and very good limit of quantification values.

MATERIALS
Product Number
Brand
Product Description

Supelco
Carbopack Adsorbent, matrix Carbopack X, 60-80 mesh, bottle of 10 g
Supelco
SPME Fiber Assembly, 65 μm PDMS/DVB, StableFlex (1 cm), needle size 24 ga, Autosampler, pk of 3, pink hub
Supelco
SPME Fiber Assembly, 65 μm PDMS/DVB, Metal Alloy (1 cm), needle size 23 ga, Autosampler, pk of 1, pink hub
Supelco
Carbopack B, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., preconditioned, pkg of 10 ea
Supelco
SPME Fiber Assembly, 7 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, green hub
Supelco
SPME Fiber Assembly, 85 μm Polyacrylate, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, white hub
Supelco
SPME Fiber Assembly, 85 μm Polyacrylate, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, white hub
Supelco
SPME Portable Field Sampler, coating CAR/PDMS
Supelco
Carbopack Adsorbent, matrix Carbopack X, 40-60 mesh, bottle of 10 g
Supelco
SPME Portable Field Sampler, coating PDMS
Supelco
SPME Fiber Assembly, 65 μm PDMS/DVB, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, blue hub
Supelco
SPME Fiber Assembly, 30 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, yellow hub
Supelco
SPME Fiber Assembly, 30 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, yellow hub
Supelco
SPME Fiber Assembly, 100 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Autosampler, pk of 3, red hub
Supelco
SPME Fiber Assembly, 65 μm PDMS/DVB, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, blue hub
Supelco
SPME Fiber Assembly, 7 μm PDMS, Fused Silica (1 cm), needle size 24 ga, Manual Holder, pk of 3, green hub
Supelco
Carbopack Adsorbent, matrix Carbopack C, 60-80 mesh, bottle of 10 g
Supelco
Carbopack B, glass TD tube, fritted, O.D. × L 1/4 in. × 3 1/2 in., unconditioned, pkg of 10 ea, matrix Carbopack
Sigma-Aldrich
Dimethyl phthalate, ≥99%
Sigma-Aldrich
Dess-Martin periodinane, 97%
Supelco
SPME Fiber Assembly, 100 μm PDMS, Metal Alloy (1 cm), needle size 23 ga, Autosampler, pk of 1, red hub
Supelco
Carbopack Adsorbent, matrix Carbopack C, 80-100 mesh, bottle of 10 g
Supelco
Carbopack B, O.D. × L 1/4 in. × 3 1/2 in., glass TD tube, fritted, Sealed with Brass Endcaps, preconditioned, pkg of 10 ea
Supelco
Carbopack B, stainless steel TD tube, O.D. × L 1/4 × 3 1/2, unconditioned, pkg of 10 ea
Supelco
FLM Carbopack X Deactivated Stainless Steel TD Tube, preconditioned, pkg of 10 tubes, O.D. × L 1/4 in. (6.35 mm) × 3 1/2 in. (89 mm)
Sigma-Aldrich
Dibutyl phthalate, 99%
Sigma-Aldrich
Dipropyl phthalate, 98%
Sigma-Aldrich
Dimethyl phthalate, ≥99%
Sigma-Aldrich
Dicyclohexyl phthalate, 99%
Sigma-Aldrich
Diisononyl phthalate, ester content ≥99 % (mixture of C9 isomers), technical grade