Effect of Stationary Phases of Gas Chromatography Columns on the Analysis of 8 Polycyclic Aromatic Hydrocarbons in a Dried Ginger (Zingiber officinale Roscoe)

Abstract

The aim of this study was to develop a simultaneous analytical method for the quantitation of 8 polycyclic aromatic hydrocarbons (PAHs) in an herbal medicinal plant, a dried ginger, using GC-MS with three GC stationary phases, including non-polar (5MS-type), mid-polar (17HT-type), and specially designed stationary phase for PAH analysis. Validations of three GC stationary phases were performed, respectively, on the base of specificity, limit of detection (LOD), limit of quantitation (LOQ), recovery, precision and accuracy. Among the three GC stationary phases, the specially designed column showed the lowest values in LOD and LOQ. In addition, interferences, such as fatty acids or fatty alcohols, as well as the targeted 8 PAH compounds were clearly separated on the column, allowing the quantification of 8 PAHs to be accurate and precise. Recoveries of 8 PAHs were in the range of 70%~120% with all three GC stationary phases. Relative standard deviations (RSD, %) of intra-day precision were in the range of 0.02%~17.18% with 5MS-type, 0.31%~7.51% with 17HT-type, and 0.09%~9.36%with specially designed capillary column for PAHs. Relative standard deviations (RSD, %) of inter-day precision were in the range of 2.51%~10.75% with 5MS-type, 1.62%~13.76% with 17HT-type, and 4.62%~12.39% with specially designed capillary column for PAHs. The accuracies of 8 PAHs were in the range of 83.59%~114.29% with 5MS-type column, 76.56%~104.96% with 17HT-type column, and 84.69%~108.41% with specially designed capillary column for PAHs.;본 연구에서는 천연물 의약품인 건강 (Zingiber officinale Roscoe, 생강의 뿌리줄기를 말린 것) 내 8가지 다환방향족탄화수소 (Polycyclic aromatic hydrocarbon, PAH)를 보다 정확하고 정밀하게 분석하기 위해 가스 크로마토그래피 (Gas chromatograpy)의 세 고정상 (5MS, 17HT, 특수제작 컬럼)을 비교 분석함으로써 8 PAHs 분석을 위한 GC-MS 동시분석법을 확립하고자 하였다. 각각의 GC 고정상은 특이성, 정성한계, 정량한계, 회수율, 정밀성, 정확성의 6가지 항목을 따라 벨리데이션이 수행되었다. 그 중 특수 제작 컬럼에서 가장 낮은 정량 및 정성한계가 도출되었다. 또한, PAHs를 분석함에 있어 방해물질로 작용하는 지방산, 지방 알코올 등은 8 PAHs와 분명하게 분리되어 보다 정확하고 정밀한 8 PAHs 정량 분석이 가능하였다. 세 고정상에서 8 PAHs 회수율은 모두 70%~120%로 나타났다. 일 내 정밀성 (RSD, %)은 0.02%~17.18%(5MS), 0.31%~7.51% (17HT), 0.09%~9.36% (특수 제작 컬럼)로 나타났다. 일 간 정밀성 (RSD, %)은 2.51%~10.75% (5MS), 1.62%~13.76% (17HT), 4.62%~12.39% (특수 제작 컬럼)으로 나타났다. 정확성은 83.59%~114.29%(5MS), 76.56%~104.96%(17HT), 4.69%~108.41% (특수 제작 컬럼)으로 나타났다.