摘要
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。
A headspace-solid phase microextraction-gas chromatography-mass spectrometry method（HS-SPME-GC-MS） was adopted for the quantitative study of 4-allylanisole,methyl eugenol,2,3,5-trimethoxytoluene,3,4,5-trimethoxytoluene,sarisan,3,5-dimethoxytoluene and safrole in mice brain,liver tissues and blood after intragastric administration of Asari Radix et Rhizoma. A VFWAXms（30 m × 0. 25 mm,0. 25 μm film thickness） capillary column and SPME fiber coated with 65 μm polydimethylsiloxane / divinylbenzene（ PDMS / DVB） were used. The calibration curves of seven volatile constituents were established to validate the method＇ s stability（ RSD 15%）,repeatability（ RSD 9. 5%）,accuracy（ RSD 22%）,relative recovery（ 87. 0%-108%） and extraction recovery（74. 9%-102%）. The validated HS-SPME-GC-MS assay was applied to determine the concentrations of seven constituents in liver,brain and blood. The detected contents were 0. 22,0. 14 μg·g^-1,0. 25 mg·L^-1（4-allylanisole）,1. 1,0. 39 μg·g^-1,0. 69mg·L1（methyl eugenol）,0. 45,0. 13 μg·g^-1,0. 54 mg·L^-1（2,3,5-trimethoxytoluene）,0. 51,0. 15 μg·g^-1,0. 45 mg·L^-1（3,4,5-trimethoxytoluene）,0. 48,0. 039 μg·g^-1,0. 69 mg·L^-1（sarisan）,2. 2,1. 2 μg·g^-1,1. 5 mg·L^-1（3,5-dimethoxytoluene） and 1. 3,0. 67 μg·g^-1,1. 1 mg·L^-1（safrole） respectively. This HS-SPME-GC-MS method is rapid and convenient,with a small sample size,and applicable for the analysis and determination of volatile constituents in traditional Chinese medicines,which provides scientific data for further studies on effective substances and toxic substances in Asari Radix et Rhizoma.
出处
《中国中药杂志》
CAS
CSCD
北大核心
2016年第2期285-293,共9页
China Journal of Chinese Materia Medica
基金
国家自然科学基金项目(81274073
81173494)
中央本级重大增减支项目(20603020102)
关键词
细辛
挥发性成分
顶空-固相微萃取-气相色谱-质谱联用技术
定量分析
生物样品检测
肝组织
脑组织
血液
Asari Radix et Rhizoma
volatile constituents
headspace-solid phase microextraction-gas chromatography-mass spectrometry
quantitative determination
biological sample detection
liver tissue
brain tissue
blood
