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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

Millipore
Bifido Selective Supplement B, suitable for microbiology
Supelco
Di-n-octyl phthalate, analytical standard
Sigma-Aldrich
Ammonium formate solution, BioUltra, 10 M in H2O
Sigma-Aldrich
Sodium phosphate dibasic dodecahydrate, tested according to Ph. Eur.
Sigma-Aldrich
5α-Androstan-17β-ol-3-one, purum, ≥99.0% (TLC)
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Magnesium sulfate solution, for molecular biology, 1.00 M±0.04 M
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5α-Androstan-17β-ol-3-one, ≥97.5%
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Diisopropyl phthalate, ≥97.0% (GC)
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Formic acid solution, BioUltra, 1.0 M in H2O
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Di-n-octyl phthalate, ≥98.0% (GC)
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Trifluoroacetic acid, ReagentPlus®, 99%
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Magnesium sulfate, ≥99.99% trace metals basis
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Diheptyl phthalate, 97%
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Sodium phosphate dibasic dodecahydrate, BioXtra, ≥99.0% (T)
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Formic acid, ≥95%, FCC, FG
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Di-n-octyl phthalate, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
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5α-Androstan-17β-ol-3-one, VETRANAL®, analytical standard
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Trifluoroacetic acid, suitable for HPLC, ≥99.0%
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Formic acid, ACS reagent, ≥96%
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Magnesium sulfate, anhydrous, free-flowing, Redi-Dri, ReagentPlus®, ≥99.5%
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Sodium phosphate dibasic dodecahydrate, meets analytical specification of Ph. Eur., BP, E339, 98.5-102.5% (T)
Plastic additive 01, European Pharmacopoeia (EP) Reference Standard
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Magnesium sulfate, anhydrous, free-flowing, Redi-Dri, reagent grade, ≥97%
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Magnesium sulfate, anhydrous, reagent grade, ≥97%
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Magnesium sulfate, anhydrous, ReagentPlus®, ≥99.5%
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Trifluoroacetic acid, puriss. p.a., suitable for HPLC, ≥99.0% (GC)
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Formic acid, ACS reagent, ≥88%
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Trifluoroacetic acid, ≥99%, for protein sequencing
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Magnesium sulfate solution, BioUltra, for molecular biology
USP
Glacial acetic acid, United States Pharmacopeia (USP) Reference Standard