Determination of 3-Monochloro-1, 2-propanediol in Acid Hydrolyzed Soysauce(Ganjang) by Gas-Chromatography with Electron Capture Detector

Gas Chromatography-Electron Capture Detector를 이용한 산분해간장중의 3-Monochloro-1, 2-propanediol 분석법에 관한 연구

To investigate the optimum condition of 3-monochloro-1, 2-propanediol(MCPD) analysis, gas chromatography with electron capture detector was used. Determination of MCPD derivatized with phenylboric acid was more effective than that of underivatized MCPD. In derivatization of MCPD with phenyl boric acid, there were no significantly different between boiling for 2min at 9$0^{\circ}C$ and vortexing for 5min at room temperature. Extrelut column was suitable for extraction of MCPD diluted in 20% NaCl solution and recovery rates were higher than direct extraction of MCPD with ethyl acetate. But, the method of direct extraction of MCPD with ethyl acetate was useful for rapid ants qualitative analysis. The sample extracted in soysauce(ganjang) was derivatized with phenylboric acid and analyzed by gas chromatography-mass selective detector. That was confirmed as MCPD-phenylboronate.

Electron capture deteotor가 장착된 gas chromatography를 이용하여 간장에서 3-monochloro-1, 2-propanediol(MCPD)의 효율적인 분석조건을 조사하였다. MCPD를 직접 분석하는 것 보다 MCPD를 phenylboric acid로 유도체화하여 분석하는 경우가 sharp한 peak를 얻을 수 있었으며, 감도도 우수하였다. 유도체화 방법을 실온에서 5분간 vortex혹은 9$0^{\circ}C$에서 20분 반응시켜 분석한 결과, R값이 각각 0.9997과 0.9977로 큰 차이를 보이지는 않았다. MCPD의 추출방법은 Extrelut 3 column을 사용하는 것이 ethyl acetate로 직접 추출하는 것보다 회수율이 월등히 높았으며, MCPD의 농노가 높을수록 회수율이 낮게 나타났다. 하지만 MCPD를 정성적으로 분석하고자 할 경우 ethyl acetate로 직접 추출하는 방법도 유효한 것으로 나타났다. 간장에 MCPD를 spiking 하고 gas chromatography-electron capture detector 및 gas chromatography-mass selective detector로 분석한 결과 sharp한 모양의 peak를 얻을 수 있었으며, mass spectrum으로 MCPD를 확인할 수 있었다.