[Determination of hexabromocyclododecanes diastereoisomers in human breast milk by HPLC-MS/MS].

Objective: A method for the determination of ac, 3 and γ-hexabromocyclododecanes (HBCDs) in human breast milk was developed by HPLC-MS/MS.

Methods: 3 -5 g human breast milk powder was spiked with '3C-HBCDs and then been extracted using Soxhlet extraction. The extract was dried and dissolved in 6ml of cyclohexane/ethyl acetate (1:1 ), then purified by gel permeation chromatography (GPC). The effluent was concentrated with rotary evaporation and then re-dissolved in hexane. 2ml of sulphuric acid was added to remove the fat for further clean-up. After drying under nitrogen, the supernatant was dissolved in 100 µl of methanol and finally determined by HPLC-MS/MS.

Results: The linear range for the three diastereoisomers of HBCDs was in 1 - 50 µg/L, with correlation coefficients ranging from 0. 9997 to 0.998. The detection limits of the three diastereoisomers ranged from 0. 12 to 0. 22 µg/L. The recoveries for three spiking levels ranged from 82. 80% to 110. 60% . The intra-day and inter-day relative standard deviations (RSD) were all less than 9. 4%.

Conclusion: The developed method was simple, convenient and sensitive. It was suitable for the determination of or, P3 and y-HBCDs in breast milk and other matrix in the future.