Determination of perchlorate in infant formula by isotope dilution ion chromatography/tandem mass spectrometry

Abstract

A sensitive and selective isotope dilution ion chromatography/tandem mass spectrometry (ID IC-MS/MS) method was developed and validated for the determination of perchlorate in infant formula. The perchlorate was extracted from infant formula by using 20 ml of methanol and 5 ml of 1% acetic acid. All samples were spiked with ¹⁸O₄ isotope-labelled perchlorate internal standard prior to extraction. After purification on a graphitised carbon solid-phase extraction column, the extracts were injected into an ion chromatography system equipped with an Ionpac AS20 column for separation of perchlorate from other anions. The presence of perchlorate in samples was quantified by isotope dilution mass spectrometry. Analysis of both perchlorate and its isotope-labelled internal standard was carried out on a Waters Quattro Ultima triple quadrupole mass spectrometer operating in a multiple reaction monitoring (MRM) negative ionisation mode. The method was validated for linearity and range, accuracy, precision, sensitivity, and matrix effects. The limit of quantification (LOQ) was 0.4 µg l⁻¹ for liquid infant formula and 0.95 µg kg⁻¹ for powdered infant formula. The recovery ranged from 94% to 110% with an average of 98%. This method was used to analyse 39 infant formula, and perchlorate concentrations ranging from <LOQ to 13.5 µg l⁻¹.

Keywords:

• liquid chromatography/mass spectrometry (LC/MS)
• in-house validation
• survey
• environmental contaminants
• infant formulae

Acknowledgments

The authors would like to thank Dr Sheryl Tittlemier and Dr Xu-liang Cao (Food Research Division, Health Canada) for providing infant formula information and samples; as well as Dr Adam Becalski, Dr Thea Rawn and Dr Rudolf Krska for providing helpful comments to the manuscript.