Research Center for Marine Ecology, the First Institute of Oceanography, SOA, QingDao, China.
J Sep Sci. 2013 Aug;36(16):2646-55. doi: 10.1002/jssc.201300184.
A simple and rapid solid-phase microextraction approach for the isolation of polycyclic aromatic sulfur heterocycles from the aromatic fraction of crude oil is described. 8-Hydroxyquinoline silica gel impregnated with palladium chloride was used as a sorbent material for extraction. Operational parameters of the extraction solvents have been evaluated and optimized. Benzothiophene, dibenzothiophene, and benzo[b]naphtho[1,2-d]thiophene and their C1-C4 alkyl derivatives were identified and quantified by GC-MS. Under optimum conditions, the limits of detection for benzothiophene, dibenzothiophene, and benzo[b]naphtho[1,2-d]thiophene were 0.277, 0.193, and 0.597 μg/g oil, respectively. The recoveries for the polycyclic aromatic sulfur heterocycles ranged from 81.5 to 92.1%, and the linear dynamic range was from 10 to 1000 ng/mL. The developed methodology was tested in the characterization of crude oil samples collected at the DY, SZ, ZH, and HC petroleum oil fields of the Bohai Sea. The results proved that SPE coupled with GC-MS is a promising tool for the quantitative analysis of polycyclic aromatic sulfur heterocycles in crude oils, especially for oil samples with low concentrations of polycyclic aromatic sulfur heterocycles.
一种从原油芳香馏分中分离多环芳烃硫杂环的简单快速固相微萃取方法。采用氯化钯浸渍的 8-羟基喹啉硅胶作为萃取的吸附材料。对萃取溶剂的操作参数进行了评估和优化。采用 GC-MS 鉴定和定量分析了苯并噻吩、二苯并噻吩和苯并[b]萘并[1,2-d]噻吩及其 C1-C4 烷基衍生物。在最佳条件下,苯并噻吩、二苯并噻吩和苯并[b]萘并[1,2-d]噻吩的检测限分别为 0.277、0.193 和 0.597 μg/g 油。多环芳烃硫杂环的回收率在 81.5%至 92.1%之间,线性动态范围为 10 至 1000 ng/mL。该方法已在渤海 DY、SZ、ZH 和 HC 油田采集的原油样品的特征描述中进行了测试。结果证明,SPE 与 GC-MS 联用是一种很有前途的工具,可用于定量分析原油中的多环芳烃硫杂环,特别是用于多环芳烃硫杂环浓度较低的油样。