论文部分内容阅读
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3min、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。
A method for the analysis of crude oil components by gas-sweep-syringe microextraction (GP-MSE) combined with GC × GC / TOFMS was established. In order to find the GP-MSE conditions suitable for the analysis of crude oil samples, the optimum conditions were obtained as follows: the sample volume was 5 mg, the extraction solvent was n-hexane 20 μL, Carrier gas flow rate 2 mL / min, heating time 3min, heating temperature 300 ℃, condensation temperature -2 ℃. The processed samples were analyzed by full 2D / MS / MS, and satisfactory results were obtained. The detection limit of the method was 34-93 μg / L with a linear correlation coefficient (R2)> 0.99. The recovery of 50 hydrocarbon compounds was between 82.0% and 107.3% with a relative standard deviation of less than 10% (n = 5) . The results showed that GP-MSE-GC × GC / TOFMS method is a new green, efficient and sensitive analytical method, which is very suitable for the analysis of volatile and semi-volatile components in crude oil.