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  • Analysis of phthalates in milk and milk products by liquid chromatography coupled to quadrupole Orbitrap high-resolution mass spectrometry.

Analysis of phthalates in milk and milk products by liquid chromatography coupled to quadrupole Orbitrap high-resolution mass spectrometry.

Journal of chromatography. A (2014-08-27)
Wei Jia, Xiaogang Chu, Yun Ling, Junrong Huang, James Chang
ABSTRACT

A new analytical method was developed and validated for simultaneous analysis of 27 phthalates in milk and milk products. Response surface methodology was employed to optimize a quick, easy, cheap, effective, rugged, and safe (QuEChERS) sample preparation method. Ultrahigh-performance liquid chromatography and electrospray ionization quadrupole Orbitrap high-resolution mass spectrometry (UHPLC/ESI Q-Orbitrap) was used for the separation and detection of all the analytes. The method was validated by taking into consideration the guidelines specified in Commission Decision 2002/657/EC and 2007/19/EC. The extraction recoveries were in a range of 90.7% to 104.6%, with coefficient of variation <5.6%. The 27 compounds behave dynamic range in the 0.1-1000μgkg(-1) concentration, with correlation coefficient >0.99. The limits of detection for the analytes are in the range 0.32-2.6μgkg(-1). This method has been successfully applied on screening of phthalates in 96 commercial milk and milk product samples.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Acetic acid-12C2, 99.9 atom % 12C
Dibutyl phthalate, European Pharmacopoeia (EP) Reference Standard
SAFC
Sodium chloride solution, 5 M
Sigma-Aldrich
Sodium chloride, BioPerformance Certified, ≥99% (titration), suitable for insect cell culture, suitable for plant cell culture
Supelco
Diisobutyl phthalate, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Supelco
Bis(2-ethylhexyl) phthalate, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Supelco
Benzyl butyl phthalate, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Supelco
Bis(2-ethylhexyl) phthalate, PESTANAL®, analytical standard
Supelco
Benzyl butyl phthalate, analytical standard
Supelco
Acetic acid, analytical standard
Supelco
Dibutyl phthalate, PESTANAL®, analytical standard
Sigma-Aldrich
Bis(2-ethylhexyl) adipate, ≥99%
Sigma-Aldrich
Sodium acetate, 99.995% trace metals basis
Sigma-Aldrich
Ammonium formate, ≥99.995% trace metals basis
Supelco
Bis(2-ethylhexyl) adipate, Selectophore, ≥99.0%
Sigma-Aldrich
Dipropyl phthalate, 98%
Sigma-Aldrich
Sodium chloride, random crystals, optical grade, 99.9% trace metals basis
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Benzyl butyl phthalate, 98%
Sigma-Aldrich
Sodium chloride, 99.999% trace metals basis
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Acetic acid, natural, ≥99.5%, FG
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Dioctyl phthalate, ≥99.5%
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Acetic acid, ≥99.5%, FCC, FG
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Sodium Acetate Anhydrous, >99%, FG
Supelco
Bis(2-ethylhexyl) adipate, 99%
Sigma-Aldrich
Sodium chloride, AnhydroBeads, −10 mesh, 99.999% trace metals basis
Sigma-Aldrich
Sodium chloride, tested according to Ph. Eur.
Supelco
Sodium chloride, reference material for titrimetry, certified by BAM, >99.5%
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Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)
Supelco
Bis(2-ethylhexyl) phthalate, Selectophore
Sigma-Aldrich
Sodium acetate solution, BioUltra, for molecular biology, ~3 M in H2O