摘要
通过研究萃取溶剂、温度、静态萃取时间和次数对萃取效率的影响,建立了加速溶剂萃取,UV-vis和LC-MS分析原油中金属卟啉的方法。结果表明,加速溶剂萃取原油中金属卟啉的最优条件为:10.3 MPa,80℃,乙腈静态萃取15 min,萃取3次。将该方法应用于孤岛原油,UV-vis结果表明,原油中钒卟啉和镍卟啉含量分别为35.95μg/g和84.48μg/g;两者均以氧化初卟啉(ETIO)和脱氧叶红初卟啉(DPEP)2种类型存在,且主要类型ETIO型分别占71.4%和80.0%。LC-MS结果显示,钒卟啉和镍卟啉的ETIO型和DPEP型系列的碳数分布范围分别是C22～C33、C25～C33和C22～C39、C28～C36,系列中含量最丰富的分别为C34-ETIO、C32-DPEP和C33-ETIO、C32-DPEP。
A method for the determination of metalloporphyrins in crude oil by ＂accelerated solvent extraction combined with UV-vis and LC-MS＂ was developed through studying the influence of extraction solvents, temperature, static extraction time and times on the extraction efficiency. The results showed that the optimal conditions to separate metalloporphyrins from crude oil by ASE were acetonitrile extracted 15 min for 3 times at 10.3 MPa and 80℃. This method was successfully applied to Gudao crude oil. UV-vis results showed that vanadium and nickel porphyrins in crude oil were 35.95 μg/g and 84.48 μg/g, they all existed in both ETIO and DPEP types, for which the contents of ETIO were 71.4% （wt） and 80.0% （wt） respectively. LC-MS results showed that C34-ETIO and C32-DPEP were the most abundant in the ETIO homologues （ C22 ～ C33 ） and DPEP homologues （C25～ C33 ） for vanadium porphyrins, whereas for nickel porphyrins, C33-ETIO and C32-DPEP were the largest abundant in the ETIO homologues （C22 ～ C39 ） and DPEP homologues （C28 ～ C36 ）.
出处
《分析试验室》
CAS
CSCD
北大核心
2013年第7期79-83,共5页
Chinese Journal of Analysis Laboratory
基金
环保部公益基金项目(201109022)资助
