热辅助在线衍生化-气相色谱法测定银杏保健品中的银杏酸  

Analysis of ginkgolic acids in dietary supplements of Ginkgo biloba by thermochemolysis-gas chromatography

作　　者：徐月婷 黄忠平[1] 王丽丽[1] 

机构地区：[1]浙江工业大学化工学院,杭州310014

出　　处：《分析试验室》2017年第9期1023-1027,共5页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金(51503182);浙江省分析测试基金(2017C37064);浙江省家具检测技术研究重点实验室资助项目(2016J01)资助

摘　　要：建立了超声辅助萃取-热辅助在线衍生化-气相色谱法测定银杏保健品中银杏酸的分析方法。在超声辅助下以甲醇萃取样品,分别吸取2.0μL衍生化试剂三甲基氢氧化硫(TMSH)与1.0μL萃取液先后加入裂解器进样杯,银杏酸在裂解炉300℃的高温下瞬间生成甲基化产物,由GC-FID(MS)分离测定。结果表明,银杏酸GA13:0在5~600 mg/L范围内线性良好,线性相关系数0.9994,检出限为1.8 mg/L(S/N=3),RSD为2.4%~2.6%(n=5)。以外标法分别测定白果种仁、白果粉饮品、银杏秋茶和春茶样品中的7种银杏酸,总含量在0.032~18.9 g/kg之间。同时,测定了银杏秋茶和春茶中银杏酸在冲泡90 min后的溶出率。白果粉饮品加标回收率在87.1%~106.1%之间。为银杏保健品中银杏酸的质量控制以及饮食的安全性评价提供了参考。A simple and sensitive method on basis of thermochemolysis-gas chromatography was established and applied into analysis of ginkgolic acids in Ginkgo biloba. Samples were extracted with methanol for 30 min assisted with ultrasonic. On-line derivatization of 1. 0 μL Ginkgo biloba sample solution at 300℃ with 2. 0 μL trimethylsulfonium hydroxide（ TMSH） allowed the analysis of methyl derivatives of ginkgolic acids. The calibration was linear over the range of 5-600 mg/L,with a correlation coefficient r = 0. 9994. The limit of detection was 1. 8 mg/L,when relative standard deviations（ n = 5） were ranged from 2. 4% to 2. 6%. The contents of ginkgolic acids in Ginkgo biloba kernels,powder drink of Ginkgo biloba kernels,Ginkgo biloba autumn tea and spring tea were ranged from 0. 032 to 18. 9 g/kg. What＇s more,the dissolution rate of ginkgolic acids brewing 90 min with boiling water of Ginkgo biloba autumn tea and spring tea was carried out. Recoveries of GA13： 0 were ranged from 87. 1%-106. 1% for the spiked powder drink of Ginkgo biloba kernels. The proposed method demonstrated a significant potential in the application of quality control and safety assessment in dietary supplements of Ginkgo biloba.

关 键 词：银杏酸 热辅助在线衍生化-气相色谱法 超声辅助萃取 银杏茶 白果 

分 类 号：TS207.3[轻工技术与工程—食品科学]