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首页> 外文期刊>Analytical methods >Oil fingerprinting analysis using commercial solid phase extraction (SPE) cartridge and gas chromatography-mass spectrometry (GC-MS)
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Oil fingerprinting analysis using commercial solid phase extraction (SPE) cartridge and gas chromatography-mass spectrometry (GC-MS)

机译：使用商业固相萃取（SPE）柱和气相色谱-质谱（GC-MS）进行油指纹分析

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This study used solid phase extraction (SPE) cartridges for rapid cleanup and fractionation of oil samples in oil fingerprinting analysis. A series of commercially available florisil cartridges, normal phase SPE cartridges, and silica gel/cyanopropyl (SiO2/C3-CN) SPE cartridges was selected for the fractionation of oil into aliphatic and aromatic hydrocarbons. The florisil cartridges and normal phase SPE cartridges can clean up the oil samples but are unable to separate them into two fractions. The SiO2/C3-CN (1 g/0.5 g) SPE cartridge successfully separated oil samples into aliphatic and aromatic fractions by eluting with 4 mL of hexane and 4 mL of dichloromethylene (DCM)/hexane (3:1, v:v), respectively. No cross-elution was observed between aliphatic and aromatic fractions when oil loading mass was less than 40 mg on the SiO2/C3-CN SPE cartridge. The relative standard deviation (RSD) of five replicates of SPE-GC-MS analysis of 5 mg of reference oil is 2.8%, 1.2%, and 6.9% for total n-alkanes, polycyclic aromatic hydrocarbons (PAHs), and biomarkers, respectively. The recoveries of six spiked deuterated surrogates were all above 95%. This SPE-GC-MS method was used for the fingerprinting analysis of various crude oils, refined petroleum products, and environmental sediment samples. The characterized target hydrocarbons included n-alkanes, unsubstituted priority PAHs and alkylated homologues, and biomarker terpanes and steranes. The concentration profiles and diagnostic ratios of target compounds are both comparable to those obtained by the conventional silica gel column-GC-MS method.
机译：这项研究使用固相萃取（SPE）柱在油指纹分析中快速净化和分离油样品。选择了一系列可商购的弗洛里西尔柱，正相SPE柱和硅胶/氰基丙基（SiO2 / C3-CN）SPE柱，以将油分馏成脂肪族和芳香族烃。弗洛里西尔柱和正相SPE柱可以清除油样，但无法将它们分成两部分。 SiO2 / C3-CN（1 g / 0.5 g）SPE柱通过用4 mL己烷和4 mL二氯亚甲基（DCM）/己烷（3：1，v：v）洗脱成功地将油样分离为脂肪族和芳香族馏分， 分别。当SiO2 / C3-CN SPE色谱柱上的油负载质量小于40 mg时，在脂族和芳族馏分之间未观察到交叉洗脱。对于总正构烷烃，多环芳烃（PAH）和生物标志物，对5 mg参考油进行5次SPE-GC-MS分析的五次重复的相对标准偏差（RSD）分别为2.8％，1.2％和6.9％。 。六个加标的氘代代用品的回收率均高于95％。该SPE-GC-MS方法用于各种原油，精炼石油产品和环境沉积物样品的指纹分析。表征的目标烃包括正构烷烃，未取代的优先PAH和烷基化的同系物以及生物标志物萜烯和甾烷。目标化合物的浓度曲线和诊断率均与常规硅胶柱-GC-MS方法获得的浓度曲线和诊断率相当。

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