- P-ISSN 1225-0163
- E-ISSN 2288-8985
본 연구에서는 다이옥신류의 정제과정으로 수동 및 자동 액체 크로마토그래피 칼럼을 이용하여 PCDDs/Fs 17종과 다이옥신과 유사한 PCB 12종의 용출 패턴을 비교, 분석하였다. 수동 알루미나 칼럼에서는 29종의 화합물이 같이 용출되어 분리되지 않았으나 자동화 칼럼의 경우 mono-ortho-PCB로부터 PCDDs/Fs 및 non-ortho PCB를 분리할 수 있었다. PAR (Precision And Recovery) 표준용액으로 조사한 다이옥신류와 PCB의 회수율은 각각 수동 액체 크로마토그래피 칼럼에서 61.9 ∼ 96.0%, 70.4 ∼ 79.0%였으며, 자동화 칼럼의 경우는 71.8 ∼ 104.5%, 61.3 ∼ 120.3% 이었다. DB-5MS 칼럼에서 분리되지 않는 #169-HxCB와 1,2,3,7,8-PeCDD은 EPA 1613 방법 중 선택이온의 비를 M+2/M+4 대신 M/M+2로 변경하여 HRGC/HRMS 분석에서 1,2,3,7,8-PeCDD와 #169-HxCB의 구분이 가능하도록 하였다.
The elution patterns of seventeen 2,3,7,8-substituted PCDDs/Fs and 12 dioxin-like PCBs were studied by both manual open columns and automatic parallel LC columns in cleanup procedure. PCDDs/Fs and non-ortho-PCBs from other mono-ortho-PCBs were separated on automatic LC column, whereas they were not separated on an open manual column. The elution study on two cleanup methods was carried out using the PAR solution of unlabeled congeners and checked the recovery of each congener. Total recoveries of cleanup fractionation were ranged between 61.9~96.0% for PCDDs/Fs and 70.4~79.0% for PCBs by manual open columns and 71.8~104.5% for PCDDs/Fs and 61.3~120.3% for PCBs by automatic parallel LC columns, respectively. Unfortunately, #169-HxCB and 1,2,3,7,8-PeCDD were not separated on DB-5MS capillary column. The ions of 1,2,3,7,8-PeCDD were selected at M/M+2 instead of M+2/M+4 suggested by EPA method 1613. It is possible to discriminate 1,2,3,7,8-PeCDD and PCB #169 in HRGC/HRMS analysis.
Washington DC, (1994.) Tetra through octachlorinated dioxins and furans by isotopic dilution HRGC-HRMS,