摘要
首次将填充毛细管高效液相色谱 毛细管气相色谱在线联用技术(μ HPLC CGC)用于分离分析八角茴香果实的挥发油成分。液相色谱选用氰基分析柱(250mm×0 32mmi d ),正己烷 乙腈 二氯甲烷(体积比为80∶8∶12)为流动相,对挥发油样品做族组分分离,得到的5个族组分被依次存放在多位储存接口内,然后不分流分别转入毛细管气相色谱仪做详细分析。气相色谱柱由10m×0 53mmi d 保留间隔柱和30m×0 53mmi d ×1 0μmSE 54分析柱组成。采用了不分流柱内进样模式以利于定量及谱图的叠加和比较。将族组成分析得到的5个气相色谱图与单独用毛细管气相色谱分析的谱图对比,发现至少分离出3种新的化学成分。
Volatile oil in Illicillm Verum Fruit was analyzed by on-line coupled packed (capillary) high performance liquid chromatography/capillary gas chromatography (μ-HPLC-CGC). A μ-HPLC column of 250 mm×0.32 mm i.d. packed with 5 μm cyano-bonded silica stationary phase was used for group separation. n-Hexane/acetonitrile/dichloromethane (80∶8∶12, (v/v)) was used as mobile phase at a flow rate of 1.8 μL/min. Five groups of eluents from the μ-HPLC were collected and stored in a multi-loop interface, which were then transferred to a capillary gas chromatograph sequentially for further analysis. A 10 m×0.53 mm i.d. retention gap connected with a 30 m×0.53 mm i.d.×1.0 μm SE-54 analytical column was used for CGC (analysis.) In-column splitless injection mode was adopted for better quantitation and manipulation of chromatograms. Five chromatograms were obtained and compared with the result of direct CGC analysis of the same sample. It was found that there were at least 3 new compounds that were not found nor separated before by conventional capillary gas chromatography/mass spectrometry method.
出处
《色谱》
CAS
CSCD
北大核心
2004年第2期101-105,共5页
Chinese Journal of Chromatography
关键词
填充毛细管液相色谱-毛细管气相色谱在线联用
八角茴香
挥发油
成分分析
packed capillary liquid chromatography/capillary gas chromatography
interface
cyano-bonded phase
volatile oil
Illicillm Verum Fruit
