Separation of hexabromocyclododecane diastereomers: Application of C18 and phenyl-hexyl ultra-performance liquid chromatography columns.
This study was performed to establish the proper liquid chromatographic conditions for the separation of hexabromocyclododecane (HBCD) diastereomers. Column selectivity towards HBCD diastereomers was evaluated for C18 and phenyl-hexyl stationary phases. First, the baseline separation of the primary HBCDs (α-, β-, and γ-HBCD) was obtained using the ultra-performance liquid chromatography (UPLC) column with C18 stationary phase chosen in most previous studies for HBCD analysis; however, co-elution of δ- and ε-HBCD with the primary HBCD diastereomers was observed. To prevent the interference from δ- and ε-HBCD, we adopted a phenyl-hexyl UPLC column to resolve the HBCD diastereomers. The phenyl-hexyl UPLC column showed significantly different selectivity for the HBCD diastereomers compared with the C18 column, which allowed the clear isolation of δ-HBCD and ε-HBCD from the primary HBCD diastereomers. In addition, by checking the retention times of all HBCD diastereomers using both C18 and phenyl-hexyl columns, we confirmed the presence of δ-, ε-, η-, and θ-HBCDs in two technical HBCD mixtures.
Korea Research Institute of Standards and Science (KRISS), 267 Gajeong-ro, Yuseong-gu, Daejeon 34113, Republic of Korea. Electronic address: songyee.baek@kriss.re.kr.
Song-Yee
SY
Baek
Korea Research Institute of Standards and Science (KRISS), 267 Gajeong-ro, Yuseong-gu, Daejeon 34113, Republic of Korea.
Sunyoung
S
Lee
Korea Research Institute of Standards and Science (KRISS), 267 Gajeong-ro, Yuseong-gu, Daejeon 34113, Republic of Korea.
Byungjoo
B
Kim
D002244:Carbon / Q000737:chemistry*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D006842:Hydrocarbons, Brominated / Q000737:chemistry* / Q000302:isolation & purification*; D013058:Mass Spectrometry; D013237:Stereoisomerism
D006842:Hydrocarbons, Brominated; C089796:hexabromocyclododecane; D002244:Carbon
10 hexabromocyclododecane diastereomers; C18 UPLC column; Phenyl-hexyl UPLC column; η-HBCD; θ-HBCD Diastereomeric analysis