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采用超声波辅助溶剂萃取技术和气相色谱-质谱(GC-MS)法,建立了烟叶中葡萄糖四酯(GTEs)类化合物的定性与定量分析方法。以甲醇为萃取溶剂,超声萃取条件经过响应面法(RSM)优化,在料液比1:28、温度32℃时,超声萃取16 min,所得萃取液经硅胶柱层析法分离并用N,O-双-三甲基三氟乙酰胺(BSTFA)-三甲基氯硅烷(TMCS)衍生后,用HP-5 MS毛细管柱分离,电子轰击源质谱检测,以全扫描模式定性分析,选择离子扫描模式定量分析。各种烟叶中共鉴定出4种GTE,分别是6-O-乙酰基-2,3,4-三-O-(3-甲基-戊酰基)-吡喃葡萄糖、6-O-乙酰基-2,3,4-三-O-戊酰基-吡喃葡萄糖、6-O-乙酰基-2,3,4-三-O-(2-甲基-丁酰基)-吡喃葡萄糖和6-O-乙酰基-2,3,4-三-O-异戊酰基-吡喃葡萄糖;4种GTE平均回收率为86.2%~97.4%,相对标准偏差为1.3%~4.0%,检出限为1.72~2.93μg/L。方法可用于11种不同类型烟叶中GTE类化合物的测定。
The methods of qualitative and quantitative analysis of GTEs in tobacco leaves were established by using ultrasonic-assisted solvent extraction and gas chromatography-mass spectrometry (GC-MS). Using methanol as extraction solvent, the ultrasonic extraction conditions were optimized by response surface methodology (RSM). When the ratio of solid to liquid was 1:28 and the temperature was 32 ℃, the extraction was carried out for 16 min by ultrasonication. The resulting extract was separated by silica gel column chromatography and eluted with N, O (BSTFA) -trimethylchlorosilane (TMCS), separated by HP-5 MS capillary column, detected by electron impact mass spectrometry, qualitative analysis by full scan mode, selective ion scan Quantitative model analysis. Four kinds of GTEs were identified in all kinds of tobacco, which are 6-O-acetyl-2,3,4-tri-O- (3-methyl- pentanoyl) -Glucopyranoside, 6-O-acetyl- O-pentanoyl-glucopyranose, 6-O-acetyl-2,3,4-tri-O- (2-methyl- butyryl) -glucopyranose and 6- O-acetyl-2,3,4-tri-O-isovaleryl-glucopyranose. The average recoveries of four GTEs ranged from 86.2% to 97.4% with relative standard deviations of 1.3% to 4.0%. The detection limits were 1.72 ~ 2.93μg / L. The method can be used for the determination of GTE compounds in 11 different types of tobacco.