HS SPME-GC/MS 를 이용한 혈액 중 유기염소계 농약의 분석법 개발
Development of an analytical method of organochlorine pesticides in human bloods using head space solid phase microextraction coupled with gas chromatography mass spectrometry
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초록
혈액 내에 축적되어 있는 유기염소계 농약을 분석하기 위한 방법으로 기존에는 액체-액체 추출 법과 고체상 추출법을 많이 사용하였으나 정제 및 많은 양의 시료 처리에 한계가 있다. 이를 극복하기 위한 방법으로 시료양이 적으며 간편한 고체상미량추출법을 사용하여 혈액 중 18종의 유기염소계 농약 의 최적 추출법을 연구하였다. 흡착조건(fiber type, 흡착시간, 흡착온도, 염석효과)과 탈착조건(탈착시간, 탈착온도) 등 최적의 추출을 위해 여러 가지의 실험조건 등을 검토한 결과, fiber는 polyacrylate 85 μm, 흡착시간은 50분, 흡착온도는 280oC, 염석효과는 NaCl 0.1 g, 탈착시간은 5분, 탈착온도는 280oC에서 최 적임을 확인하였다. 정확도, 정밀도 및 검출한계에 대한 타당성을 최적 실험조건에서 조사한 결과, 검출 한계는 0.05~0.20 ng/mL, 정밀도는 5.59~13.39%, 정확도는 -0.5%~24.5%의 범위인 것으로 확인되었다.
Abstract
The analytical method of extracting compounds from human blood to examine accumulated organochlorine pesticides (OCPs) has been widely used the traditional liquid-liquid extraction (LLE) method and solid-phase extraction (SPE) method, yet these methods have certain limitations in purification and usafe of a large amount of sample. In order to overcome the se problems reside in these, solid-phase microextraction (SPME), known as a highly efficient extration method with less samples and relatively simple, was employed to collect 18 different kinds of OCPs in blood as extraction method in this study. To optimize extraction method, we examine various experimental SPME-parameters such as adsorption (fiber type, adsorption time, adsorption temperature, salting out effect), and desorption (desorption time, desorption temperature etc.). From the experimental results, the optimal conditions are as follows: fiber was polyacrylate with 85 μm, adsorption time was for 5 min, adsorption optimum temperature was at 280oC, and salting out effect was NaCl with 0.1 g. MDL, precision and accuracy was in the ranges of 0.05~0.20 ng/mL, 5.59~13.39%, respedively, and accuracy was -0.5% ~24.5% for all OCPs
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