US EPA

4216020 

Journal Article 

Determination of phthalate diesters and monoesters in human milk and infant formula by fat extraction, size-exclusion chromatography clean-up and gas chromatography-mass spectrometry detection 

Del Bubba, M; Ancillotti, C; Checchini, L; Fibbi, D; Rossini, D; Ciofi, L; Rivoira, L; Profeti, C; Orlandini, S; Furlanetto, S 

2018 

Yes 

Journal of Pharmaceutical and Biomedical Analysis
ISSN: 0731-7085
EISSN: 1873-264X 

148 

6-16 

English 

28946042 

10.1016/j.jpba.2017.09.017 

WOS:000417771700002 

A sensitive and reliable analytical method was developed for the simultaneous determination of five phthalate diesters and corresponding monoesters in human milk samples and infant formulas. The method involved a liquid-liquid extraction with a CH2Cl2/CH3OH/NaCl 30% 2/1/0.5 (v/v/v) mixture, the clean-up of the extract by size-exclusion chromatography (swelling and elution solvent: cyclohexane/ethyl acetate 9/1v/v), the derivatization of monoesters by trimethylsilyl-diazomethane and instrumental analysis by gas chromatography coupled with mass spectrometry. Recovery was in the range of 83-115% and precision was found between 9% and 21%. For phthalate diesters, method detection limits (MDLs) ranged from hundreds of ng/kg to 4.2μg/kg on a fresh weight milk (f.w.) basis, depending on blank contribution evaluated in matrix. Lower MDLs (0.03-0.8μg/kg f.w.) were achieved for corresponding monoesters. The proposed method was applied to the determination of target compounds in nine human milk samples and four infant formulas, confirming their presence in all samples. However, a generally higher contamination was assessed in artificial milk than in breast milk samples.