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作 者:李晶[1,2] 耿永勤 魏玉玲[1] 陈建华[1] 邓立花[3] 徐济仓[1]
机构地区:[1]云南烟草科学研究院 [2]工业控制技术国家重点实验室浙江大学智能系统与控制研究所,杭州市浙大路38号310058 [3]云南农业职业技术学院,昆明市茭菱路128号650031
出 处:《光谱实验室》2013年第5期2487-2491,共5页Chinese Journal of Spectroscopy Laboratory
基 金:云南中烟公司科研资助项目(No.2012JC05)
摘 要:建立了气相色谱串联质谱(G C-M S)准确、快速测定香精香料中仲丁醇、富马酸二甲酯、咪唑和芝麻酚的分析方法。样品经甲醇超声提取15min后,通过Agilent DB-WAX(0.25mm×30m×0.25Lm)色谱柱分离,质谱进行定性,外标法对于4种目标物质进行定量分析。实验结果表明,在0.5—20mg/L的范围内,4种物质具有较好的线性,各待测物质的线性相关系数均大于0.9990,检出限为0.02—0.12mg/L,在1,5mg/L和10mg/L 3个加标水平条件下,4种禁限用物质的平均回收率为88.0%—113.1%,相对标准偏差为0.32%—6.53%。该方法前处理简单,灵敏度高,线性相关性好,重复性佳,可以满足香精香料中4种物质的同时检测。A gas chromatography coupled with mass spectrometry as detector (GC-MS) was established for the separation and determination of 4 substances (s-butanol, dimethyl fumarate, imidazole,sesamol) in flavor and fragrant samples. After extracted by HPLC methanol, the target compounds were separated on an Agilent DB-WAX capillary column (0.25mm×30m×0.25μm). Selected ion monitoring (SIM) mode of GC-MS was used in quantitation. It's exhibited that there was a good linear relationship (〉0. 9990) ranged from 0. 5 to 25mg/L and the limits of detection was in range of 0. 02--0.12mg/L. The average recoveries at three levels were in the range of 88.0%-- 113.1% with the relative standard deviations (RSD)ranged from 0. 32% to 6. 53%. This simple method can be used to determine 4 substances in flavor and fragrant samples simultaneously.
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