GC/MS의 Scan/SIM Mode 동시 분석에 의한 혈액 중 유기인계 농약의 분석
Analysis of 25 Organophosphorus Pesticides in Blood by Synchronous Scan/SIM Mode GC/MS
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초록
기체크로마토그래프-질량분석법(GC/MS)의 Scan 및 SIM mode 동시 분석법을 이용하여 25종의유기인계 농약성분을 선택적으로 분석하였으며 추출은 고체상미량 추출법으로 Oasis HLB 카트리지를사용하였다. 전자충격으로 분석대상 화합물을 이온화시켰으며 Scan mode와 3개의 특징 이온을 이용한SIM mode로 각각의 크로마토그램을 얻었다. GC/MS의 SIM mode의 검출정도는 Scan mode 보다 좋으나특정 목적 성분이외는 어떤 정보도 얻을 수 없는 단점이 있기 때문에 Scan mode를 동시에 얻음으로서 이러한 단점을 보완할 수 있었으며 SIM mode를 이용하여 25종의 유기인계 농약성분에 대하여 시험법에 대한 유효화를 실시하였다. 혈액에서 25종의 유기인계 농약 성분의 회수율은 62.8% ~ 98.0%였으며 검출한계및 정량한계는 각 각 5 ng/mL ~ 10 ng/mL 및 10 ng/mL ~ 20 ng/mL로 나타났다. 직선성은 20 ng/mL의 농도로부터 유기인계 농약의 성분에 따라 250 ng/mL ~ 2500 ng/mL에서 r2 = 0.99 이상의 직선성을 보였으며시험 간 및 시험내의 정확도와 정밀도가 유효화 조건을 충족하였다.
Abstract
This study described a specific and sensitive method for the determination of 25 organophosphorus pesticides in blood, using a rapid solid-phase extraction(SPE) procedure with Oasis HLB cartridges and gas chromatography-mass spectrometry in synchronous scan and selective ion monitoring(SIM) modes. The ionization was carried out by electron impact and acquisition in scan and SIM mode identifying three specific ions per component. Scan GC/MS analysis is a commonly employed data collection mode for pesticides to acquire both qualitative and quantitative information and SIM analysis provides more sensitivity than the scan mode does, but does not give any information regarding non-target analytes. So combining these two analysis modes makes a more powerful analysis method that can give synchronously both qualitative and quantitative information. Extraction recoveries were satisfactory and ranged between 62.8 and 98.0% in blood. Limits of detection (LODs) ranged from 5 to 10 ng/mL and limites of quantitation (LOQs) ranged from 10 to 20 ng/ mL in blood. An excellent linearity was observed, r2 > 0.99, from 20 up to 250-2500 ng/mL for the components of organophosphorus pesticides. Intra- and inter-assay precision and accuracy were satisfactory for the most of 25 organophosphorus pesticides analyzed.
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