Determination of Bisphenol A and 4-Nonylphenol in Human Milk Using Alkaline Digestion and Cleanup by Solid-Phase Extraction

Abstract

A highly sensitive and selective method based on alkaline digestion for the simultaneous determination of bisphenol A (BPA) and 4-nonylphenol (NP) was developed. The method consists of digestion of the matrix with ethanolic KOH, extraction with diethyl ether under a mild alkaline condition, cleaning with successive aminopropyl (NH2) cartridges and derivatization followed by a GC-MS analysis. The assay accuracies, expressed as recoveries, were 82 -113% for BPA and 89 -97% for NP. The limits of detection of BPA and NP were 0.09 ng/g and 0.50 ng/g, respectively. The procedure will be reliable for the trace analysis of BPA and NP in human milk, since alkaline digestion can diminish their documented association with protein.

Measuring environmental phenols and chlorinated organic chemicals in breast milk using automated on-line column-switching–high performance liquid chromatography–isotope dilution tandem mass spectrometry

“…Compared with other methods [10,13], our on-line SPE-HPLC-MS/MS method provides similar sensitivity, precision, and accuracy, without complicated and timeconsuming sample preparation. Our method can be used for quick, accurate, and cost-effective analysis of large numbers of samples in epidemiologic studies to assess the prevalence of infant exposure to selected phenols and chlorinated organic chemicals via breastfeeding.…”

“…Interest in monitoring breast milk for environmental contaminants is increasing because breast milk is the main route of exposure to environmental chemicals for breastfed infants. Methods that have been reported use several analytical techniques to measure environmental phenols in milk [10][11][12][13]. BPA was measured by high performance liquid chromatography (HPLC) with column-switching and fluorescence detection [11]; and by alkaline digestion followed by solid-phase extraction (SPE), derivatization, and detection by gas chromatography-mass spectrometry (GC-MS) [10].…”

“…Methods that have been reported use several analytical techniques to measure environmental phenols in milk [10][11][12][13]. BPA was measured by high performance liquid chromatography (HPLC) with column-switching and fluorescence detection [11]; and by alkaline digestion followed by solid-phase extraction (SPE), derivatization, and detection by gas chromatography-mass spectrometry (GC-MS) [10]. Chlorophenols were measured using solid-phase microextraction coupled with GC-electron capture detection [13].…”

Determination of bisphenol A and related substitutes/analogues in human breast milk using gas chromatography-tandem mass spectrometry

“…Data have been published regarding for instance the determination of bisphenol AF in both serum and urine of rats [9] or BPS, BPF, and BPB in human urine [10][11][12][13]. Several authors have also reported different analytical methods for the determination of BPA in breast milk [14][15][16][17][18][19][20][21][22][23]. Kuruto-Niwa et al [14] and Migeot et al [22] reported data for the determination of BPA in colostrum samples.…”

“…This analytical method has been widely used for the determination of BPA in different biological matrices in the framework of various cohort population studies. Samanidou et al [20] and Otaka et al [21] reported analytical methods based on MSPD and alkaline digestion, respectively, for the determination of BPA in breast milk samples. Cariot et al also reported an on-line SPE-ultra high-performance liquid chromatography (UHPLC)-MS/MS method from a 500-μL test sample with a limit of quantification (LOQ) of 0.4 ng mL −1 [18].…”