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采用顶空-固相微萃取-气相色谱-质谱联用技术(HS-SPME-GC-MS)对灌胃给药细辛后吸收入小鼠体内的细辛活性成分4-烯丙基苯甲醚、甲基丁香酚、2,3,5-三甲氧基甲苯、3,4,5-三甲氧基甲苯、细辛素、3,5-二甲氧基甲苯和黄樟醚进行了定量研究。采用VF-WAXms毛细管柱(0.25 mm×30 m,0.25μm)和SPME萃取头PDMS/DVB(65μm),建立了7个成分的标准曲线,验证了该方法稳定性(RSD<15%)、重复性(RSD<9.5%)、精密度(RSD<22%)、相对回收率(87.0%~108%)和提取回收率(74.9%~102%),并使用验证后的方法确定了7个主要吸收成分的量,在给药后小鼠肝、脑和血液中检测到的质量分数分别为4-烯丙基苯甲醚0.22,0.14μg·g-1,0.25 mg·L-1;甲基丁香酚1.1,0.39μg·g-1,0.69 mg·L-1;2,3,5-三甲氧基甲苯0.45,0.13μg·g-1,0.54 mg·L-1;3,4,5-三甲氧基甲苯0.51,0.15μg·g-1,0.45 mg·L-1;细辛素0.48,0.039μg·g-1,0.69 mg·L-1;3,5-二甲氧基甲苯2.2,1.2μg·g-1,1.5 mg·L-1;黄樟醚1.3,0.67μg·g-1,1.1 mg·L-1。结果表明HS-SPME-GC-MS分析方法适合于中药中挥发性成分在体内的分析测定,样品用量少,快速简便;含量测定数据为进一步认识细辛药材有效物质和毒性物质提供了科学资料。
Gas chromatography-mass spectrometry (HS-SPME-GC-MS) was used for the determination of 4-allylbenzoic acid Ether, methyl eugenol, 2,3,5-trimethoxytoluene, 3,4,5-trimethoxytoluene, asarubicin, 3,5-dimethoxytoluene and safrole were quantitatively studied. A standard curve of seven components was established using a VF-WAXms capillary column (0.25 mm × 30 μm, 0.25 μm) and a PDME / DVB (65 μm) SPME extraction head to verify the stability of the method (RSD <15% (RSD <9.5%), precision (RSD <22%), relative recoveries (87.0% -108%) and extraction recoveries (74.9% -102%). The mass fraction of the absorbed components in the liver, brain and blood of the mice after administration was respectively 0.22, 0.14 μg · g-1 and 0.25 mg · L-1 for 4-allyl anisole, Eugenol 1.1, 0.39 μg · g-1, 0.69 mg · L -1; 2,3,5-trimethoxytoluene 0.45, 0.13 μg · g -1, 0.54 mg · L -1; Trimethoxytoluene 0.51, 0.15μg · g-1, 0.45 mg · L-1; asarone 0.48, 0.039μg · g-1, 0.69 mg · L -1; 3,5-dimethoxytoluene 2.2, 1.2μg · g-1, 1.5 mg · L-1; safrole 1.3, 0.67μg · g-1, 1.1 mg · L-1. The results showed that the method of HS-SPME-GC-MS was suitable for the in vivo analysis of volatile components in traditional Chinese medicine, with less sample amount and quickness and convenience. The content determination data provided scientific data for further understanding the effective substances and toxic substances of Asarum .