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.
出处
《分析试验室》
CAS
CSCD
北大核心
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
关键词
烟叶
超声萃取
响应面法
葡萄糖四酯
气相色谱-质谱
Tobacco
Ultrasonic extraction
Response surface methodology
Glucose tetra-esters （ GTE ）
Gas chromatography-mass spectrometry （GC-MS）
