静态顶空-GC/MS技术分析浸膏中的溶剂残留  

Residual solvent analyses in plant extracts by static headspace gas chromatographymass spectrometry

作　　者：卢斌斌[1] 张璟琳[2,3] 曾世通[1] 孙世豪[1] 李娟[2] 孙宝国[2] 黄明泉[2] 

机构地区：[1]中国烟草总公司郑州烟草研究院 [2]北京工商大学北京食品营养与人类健康高精尖创新中心,北京市海淀区阜成路11号100048 [3]北京工商大学理学院,北京市海淀区阜成路11号100048

出　　处：《烟草科技》2016年第10期60-65,共6页Tobacco Science & Technology

基　　金：国家自然科学基金项目"中国传统菜肴中氯丙醇酯的形成机理与消长规律研究"(31471665);北京市属高等学校高层次人才引进与培养计划项目(CIT&TCD 201404034)

摘　　要：为研究浸膏类添加剂中的溶剂残留,采用静态顶空进样结合气质联用仪对5种浸膏（枸杞浸膏、山楂浸膏、杭白菊浸膏、茉莉浸膏、桂花浸膏）共15个样品中的27种残留溶剂进行了定性定量分析。静态顶空条件为60℃平衡15 min,进样体积为0.40 mL,利用NIST谱库和标准品定性,外标法定量。结果表明：（1）该方法对12种溶剂定量的线性范围良好,线性相关系数均大于0.99,回收率在78.60%~120.80%之间,相对标准偏差为11.50%~16.94%。（2）枸杞浸膏、山楂浸膏、杭白菊浸膏和桂花浸膏（GH1）中的主要残留溶剂为乙醇;桂花浸膏（GH2、GH3）和茉莉浸膏中的主要残留溶剂为甲基环戊烷、正己烷、异己烷和环己烷。To study the levels of solvent residues in plant extracts, 27 residual solvents in 15 samples of 5 types of extracts（medlar, hawthorn, chrysanthemum, jasmine, osmanthus） were qualitatively and quantitatively analyzed by static headspace（HS） combined with GC-MS. The samples were dissolved in headspace vials and kept warm at 60 ℃ for 15 min. A sample of 0.40 mL headspace volatiles was injected into GC-MS using external standard for peak identification. NIST database and standards plus internal standards were used for qualitatively and quantitatively analyses, respectively. The results showed that： 1） The linear range of quantitatively analysis for 12 solvents was satisfactory with the r values all above 0.99, and the recovery and RSD values were in the range of 78.60%-120.80% and 11.50%-16.94%, respectively. 2） Ethyl alcohol was the main residual solvent in medlar, hawthorn, chrysanthemum, and osmanthus（GH1） extracts. The main residual solvents in the other osmanthus extracts（GH2, GH3） and jasmine extracts were methylcyclopentane, n-hexane,isohexane and cyclohexane.

关 键 词：静态顶空 溶剂残留 浸膏 烟草添加剂 气质联用 质量安全 

分 类 号：TQ656.5[化学工程—精细化工]