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. 2021 Jun 16;26(12):3664.
doi: 10.3390/molecules26123664.

Confirmatory Analysis of Per and Polyfluoroalkyl Substances in Milk and Infant Formula Using UHPLC-MS/MS

Ovokeroye A Abafe  1   2 , Linda R Macheka  1   3 , Joshua O Olowoyo  3
Affiliations

Confirmatory Analysis of Per and Polyfluoroalkyl Substances in Milk and Infant Formula Using UHPLC-MS/MS

Ovokeroye A Abafe et al. Molecules. .

Abstract

An ultra-high performance liquid chromatography tandem mass spectrometry method was developed and validated for the sensitive determination and unambiguous confirmation of residues of per and polyfluorinated alkyl substances (PFAS) in breastmilk, retail milk and infant formulas following two sample preparation methods. Sample pre-treatment was carried out by a simplified QuEChERS method without requiring dSPE or any further clean-up. The method was validated in accordance with the requirements of Commission Decision 657/2002/EC with slight modifications. The method displayed good linearity with R2 ranging from 0.9843-0.9998 for all target PFAS. The recovery and within-laboratory reproducibility of the method (n = 63) were in the range 60-121% and 5-28%, respectively. The decision limit, detection capability and limit of quantitation ranged from 30-60 ng kg-1 to 40-100 ng kg-1 and 5-50 ng kg-1, respectively. Acceptable matrix effect values in the range -45-29% were obtained with uncertainty of measurement lower than 25% for all target PFAS. The method displays its suitability for the sensitive and high-throughput confirmatory analysis of C4-C14 PFAS in breastmilk, dairy milk and infant formulas.

Keywords: QuEChERS; UHPLC–MS/MS; breastmilk; confirmatory; infant formula; liquid–liquid extraction; retail milk.

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Conflict of interest statement

The authors declare no conflict of interest.

Figures

Figure 1
Figure 1
Selectivity of per and polyfluorinated alkyl substances (PFAS) in milk: (a) TIC of milk matrix blank; (b) TIC of spiked milk.
Figure 1
Figure 1
Selectivity of per and polyfluorinated alkyl substances (PFAS) in milk: (a) TIC of milk matrix blank; (b) TIC of spiked milk.
Figure 2
Figure 2
Recovery of PFAS using varying sample weight.
Figure 3
Figure 3
Recovery (n = 3) of PFAS in milk using the simplified QuEChERS, liquid–liquid and Oasis HLB SPE cartridge.
Figure 4
Figure 4
(a) Total ion chromatogram of 10,000 ng kg−1 PFAS spiked in milk in MRM acquisition mode. (b) Improved total ion chromatogram of 10,000 ng kg−1 PFAS spiked in milk in time-managed MRM acquisition mode.
Figure 5
Figure 5
Recovery of PFAS in dairy milk, infant formula and breastmilk.
See this image and copyright information in PMC

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