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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

Supelco
Benzyl butyl phthalate, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
SAFC
Sodium chloride solution, 5 M
Sigma-Aldrich
Acetic acid, glacial, ACS reagent, ≥99.7%
Dibutyl phthalate, European Pharmacopoeia (EP) Reference Standard
USP
Sodium acetate, United States Pharmacopeia (USP) Reference Standard
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Sodium chloride, Vetec, reagent grade, 99%
Sigma-Aldrich
Sodium acetate, Vetec, reagent grade, 98%
Sigma-Aldrich
Acetic acid, glacial, puriss., 99-100%
Sigma-Aldrich
Acetic acid, glacial, puriss., meets analytical specification of Ph. Eur., BP, USP, FCC, 99.8-100.5%
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Acetic acid, glacial, ≥99.99% trace metals basis
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Sodium acetate, anhydrous, free-flowing, Redi-Dri, ACS reagent, ≥99.0%
Sigma-Aldrich
Acetic acid, glacial, ReagentPlus®, ≥99%
Sigma-Aldrich
Sodium acetate, LR, anhydrous, ≥98%
Sigma-Aldrich
Sodium acetate, suitable for HPLC, ≥99.5%
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Sodium chloride, AR, ≥99.9%
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Acetic acid, LR, ≥99.5%
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Dibutyl phthalate, LR, ≥98%
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Acetic acid, AR, ≥99.8%
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Dibutyl phthalate, AR, ≥99%
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Acetic acid, suitable for HPLC, ≥99.8%
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Ammonium formate, reagent grade, 97%
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Acetic acid, glacial, puriss. p.a., ACS reagent, reag. ISO, reag. Ph. Eur., ≥99.8%
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Sodium acetate, ACS reagent, ≥99.0%
Supelco
Diisobutyl phthalate, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Sigma-Aldrich
Sodium acetate, puriss. p.a., ACS reagent, reag. Ph. Eur., anhydrous
Supelco
Bis(2-ethylhexyl) phthalate, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Sigma-Aldrich
Acetic acid solution, suitable for HPLC
Supelco
Dibutyl phthalate, certified reference material, TraceCERT®, Manufactured by: Sigma-Aldrich Production GmbH, Switzerland
Sigma-Aldrich
Sodium acetate, anhydrous, ReagentPlus®, ≥99.0%
Supelco
Sodium chloride, Pharmaceutical Secondary Standard; Certified Reference Material