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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

Dibutyl phthalate, European Pharmacopoeia (EP) Reference Standard
Supelco
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Dibutyl phthalate, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
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Diisobutyl phthalate, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
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Acetic acid-12C2, 99.9 atom % 12C
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Sodium chloride, BioPerformance Certified, ≥99% (titration), suitable for insect cell culture, suitable for plant cell culture
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Bis(2-ethylhexyl) adipate, 99%
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Sodium chloride-35Cl, 99 atom % 35Cl
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Sodium chloride, random crystals, optical grade, 99.9% trace metals basis
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Diphenyl phthalate, 99%
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Sodium acetate, 99.995% trace metals basis
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Dibutyl phthalate, 99%
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Diisononyl phthalate, ester content ≥99 % (mixture of C9 isomers), technical grade
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Bis(2-ethylhexyl) adipate, ≥99%
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Benzyl butyl phthalate, analytical standard
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Acetic acid, analytical standard
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Sodium chloride, BioUltra, for molecular biology, ≥99.5% (AT)
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Sodium chloride, tested according to Ph. Eur.
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Sodium acetate, anhydrous, BioUltra, for luminescence, for molecular biology, ≥99.0% (NT)
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Ammonium formate, eluent additive for LC-MS, LiChropur, ≥99.0%
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Ammonium formate, BioUltra, ≥99.0% (calc. based on dry substance, NT)
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Sodium acetate solution, BioUltra, for molecular biology, ~3 M in H2O
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Sodium chloride, reference material for titrimetry, certified by BAM, >99.5%
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Bis(2-ethylhexyl) phthalate, Selectophore
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Sodium chloride, 99.999% trace metals basis
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Sodium Acetate Anhydrous, >99%, FG
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Dipropyl phthalate, 98%
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Bis(2-ethylhexyl) adipate, Selectophore, ≥99.0%
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Ammonium formate, ≥99.995% trace metals basis