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摘要: 依次用石油醚、CS2、CH2Cl2、丙酮和甲醇在索氏萃取器中萃取了神木半焦粉末, 得到了五级萃取物(E1-5) 和最终的萃余物, 总萃取率为1.76%。分别用气相色谱/质谱联用仪(GC/MS)、大气压固体探针/飞行时间质谱仪(ASAP/TOF-MS) 和电喷雾电离/飞行时间质谱仪(ESI/TOF-MS) 分析了各级萃取物。用GC/MS分析的结果表明, 在E1中C15-24的直链烷烃和E2中3与4环的芳烃比较丰富, 在E3-5中含杂原子有机化合物较丰富, 特别是E4和E5中含氧有机化合物的含量最高。与用GC/MS分析的结果相比, 用ASAP/TOF-MS和ESI/TOF-MS从E3-5中检测出更多的含杂原子有机化合物。Abstract: Shenmu char powder (SCP) was sequentially extracted with petroleum ether, carbon disulfide, dichloromethane, acetone, and methanol in a Soxhlet extractor to obtain extracts 1-5 (E1-5) and final residue. The total extract yield of SCP is 1.76%. All the extracts were characterized with gas chromatograph/mass spectrometer (GC/MS), atmospheric solid analysis probe/time-of-flight mass spectrometer (ASAP/TOF-MS), and electrospray ionization/time-of-flight mass spectrometer (ESI/TOF-MS). Normal alkanes with C15 to C24 and arenes with 3 and 4 rings are predominant in E1 and E2, respectively, while more heteroatom-containing organic species were identified in E3-5. Organooxygen compounds are the most abundant in E4 and E5 based on analysis with GC/MS. Much more heteroatom-containing organic compounds were detected in E3-5 with ASAP/TOF-MS and ESI/TOF-MS than with GC/MS.
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Key words:
- char powder /
- Soxhlet extraction /
- extracts /
- compositional features
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Figure 3 Distribution of group components in the extracts according to GC/MS analysis
: HACOSs; : arenes; : alkenes; : alkanes
Figure 7 Distribution of group components detected in the extracts according to analysis with ASAP-TOF/MS.
Figure 8 Distribution of group components detected in the extracts according to analysis with ESI-TOF/MS.
Table 1 Proximate and ultimate analyses of SCP
Proximate analysis w/% Ultimate analysis wdaf/% Mad Ad Vdaf C H N S Oa 5.11 21.23 12.15 78.29 1.22 0.87 0.56 19.06 a: by difference 
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Table 2 Sulfur-containing species detected in the extracts with GC/MS
Peak Name Detected in E1 E2 E3 E4 E5 1 2, 6-dimethyl-4H-pyran-4-thione × 2 3-methyl-2, 3-dihydrobenzo[ b]thiophene × 3 hexathiane × × 4 dibenzo[ b, d]thiophene × 5 octathiocane × 6 octahydro-2 H, 2' H-4, 4'-bithiopyran × 7 1, 3, 2-benzodioxathiole 2-oxide × 8 1, 2, 3, 4-tetrahydropyrimido[4', 5':4, 5]thieno[2, 3-c]isoquinolin-8-amine × 9 (Z)-2-(3, 6-dimethylbenzo[ d]thiazol-2(3 H)-ylideneamino) ethanol ×
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