CAJ | 학술논문

建立了气流吹扫-注射器微萃取（GP-MSE）与全二维气相色谱/飞行时间质谱（GC×GC/TOFMS）联用分析原油成分的方法。为了找到适用于原油样品分析的 GP-MSE条件，用饱和烃混合标准溶液和15种芳烃的混合标准溶液进行了条件优化，得到的最佳条件如下：取样量5 mg、萃取溶剂正己烷20μL、载气流速2 mL/min、加热时间3 min、加热温度300℃、冷凝温度-2℃。处理后的样品在全二维色谱/飞行时间质谱上进样分析，得到了满意结果。方法的检出限为34~93μg/L，线性相关系数（R2）﹥0.99，对50种烃类化合物的回收率在82.0％~107.3％之间，相对标准偏差＜10％（n＝5）。结果表明 GP-MSE-GC×GC/TOFMS法是一种新型绿色、高效、灵敏的分析方法，非常适合原油中挥发性与半挥发性组分的分析。
건립료기류취소-주사기미췌취（GP-MSE）여전이유기상색보/비행시간질보（GC×GC/TOFMS）련용분석원유성분적방법。위료조도괄용우원유양품분석적 GP-MSE조건，용포화경혼합표준용액화15충방경적혼합표준용액진행료조건우화，득도적최가조건여하：취양량5 mg、췌취용제정기완20μL、재기류속2 mL/min、가열시간3 min、가열온도300℃、냉응온도-2℃。처리후적양품재전이유색보/비행시간질보상진양분석，득도료만의결과。방법적검출한위34~93μg/L，선성상관계수（R2）﹥0.99，대50충경류화합물적회수솔재82.0％~107.3％지간，상대표준편차＜10％（n＝5）。결과표명 GP-MSE-GC×GC/TOFMS법시일충신형록색、고효、령민적분석방법，비상괄합원유중휘발성여반휘발성조분적분석。
A novel sample pretreatment method, gas purge micro-syringe extraction ( GP-MSE), coupled to comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry( GC × GC/TOFMS ) has been developed for the characterization of volatile and semi-volatile compounds in crude oils. In the sample pretreatment process,the analytes were carried to the microsyringe barrel by inert gas,and at the same time,trapped by an organic sol-vent. The whole process of extraction takes less than 10 min,and only 20 μL of organic solvent was needed. Using two custom standard solutions containing alkanes and polycyclic aromatic hydrocarbons( PAHs),the influences of the extraction conditions were investigated. The opti-mized conditions were as follows:5 mg crude oil,20 μL hexane( extraction solvent),extrac-tion for 3 min at 300 ℃,condensation temperature set at -2 ℃,gas flow rate set at 2 mL/min. Under the optimized conditions,a real crude oil sample was extracted and then analyzed in de-tail. It showed that the proposed method was very effective in simultaneously analyzing the nor-mal and branched alkanes,cycloalkanes,aromatic hydrocarbons,and biomarkers of crude oil such as steranes and terpanes. The recoveries obtained ranged from 82. 0% to 107. 3% and the detection limits ranged from 34 to 93 μg/L. The correlation coefficients( R 2 )were more than 0. 99. The relative standard deviations( RSDs,n=5)for all the analytes were below 10%. The results indicate that the proposed method is suitable for the characterization of volatile and semi-volatile compounds in crude oils with easy operation,high sensitivity and efficiency.