超声萃取-气相色谱-质谱法测定烟叶中的葡萄糖四酯  

Determination of glucose tetra-esters in tobaccos by ultrasonic extraction coupled with gas chromatographymass spectrometry

作　　者：贾春晓[1] 王瑞玲[1] 王莹莹[1] 毛多斌[2] 

机构地区：[1]郑州轻工业学院材料与化学工程学院,郑州450002 [2]郑州轻工业学院烟草科学与工程学院,郑州450002

出　　处：《分析试验室》2013年第12期55-60,共6页Chinese Journal of Analysis Laboratory

基　　金：国家自然基金项目(21176229);中国烟草总公司卷烟增香保润重大科技专项(110201101025(BR-07))资助

摘　　要：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32c（=时，超声萃取16min，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-5MS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。A method was developed for the qualitative and quantitative determination of glucose tetra-esters （GTEs） in tobaccos by gas chromatography-mass spectrometry （GC-MS） after ultrasonic extraction. The ultrasonic extraction parameters were optimized by response surface methodology（RSM）. The optimal conditions were to use methanol as the extraction solvent within 16 min at 32℃ and the solid liquid ratio was 1：28. The GTEs extracted from tobaccos were cleaned up by a silica column and derived with N, O-bis （trimethylsilyl） trifluoroacetamide （BSTFA）-trimethylchlorosilane （TMCS）. The GTE derivatives were separated by gas chromatography using a HP -5MS capillary column and detected by mass spectrometry. Full scan mode and SIM mode were used for the qualitative and quantitative analysis, respectively. Four kinds of GTEs were identified from tobaccos, and they were 6-O-acetyl - 2,3,4-tri-O - （3-methylbutyryl） -glucopyranose, 6-O-acetyl - 2,3,4- tri -O -valeryl -glucopyranose, 6-O-acetyl - 2,3,4-tri -O -isoamyl-glucopyranose and 6-O-acetyl - 2,3,4-tri -O - （ 3 - methylvaleryl） -glucopyranose. The average recoveries of the four GTEs in the range from 86. 2% to 97.4% （ n = 5 ）, the relative standard deviations were between 1.3% and 4.0%, and the detection limits were in the range of 1.72 - 2.93 μg/L. The method for the detection of four GTEs in 11 tobacco samples was sensitive and highly reproducible with satisfactory recoveries.

关 键 词：烟叶 超声萃取 响应面法 葡萄糖四酯 气相色谱-质谱 

分 类 号：O657.63[理学—分析化学]