气相色谱-火焰离子化检测法和气相色谱-质谱法检测蜂蜜中17-三十五烯含量

Determination of 17-pentatriacontene in honey by gas chromatography-flame ionization detection and gas chromatography-mass spectrometry

中文关键词:  17-三十五烯  中蜂蜂蜜  意蜂蜂蜜  特征成分  气相色谱-火焰离子化检测法  气相色谱-质谱法

英文关键词:17-pentatriacontene  Apis cerana honey  Apis mellifera honey  characteristic compounds  gas chromatography-flame ionization detection  gas chromatography-mass spectrometry

中文摘要:

      目的 建立气相色谱-火焰离子化检测法(gas chromatography-flame ionization detection, GC-FID)和气相色谱-质谱法(gas chromatography-mass spectrometry, GC-MS)测定蜂蜜中17-三十五烯含量的方法。方法 样品经水溶解, 石油醚提取, 弗罗里硅土柱固相萃取净化, DB-5MS色谱柱(15 m×0.25 mm, 0.25 μm)分离, 分别采用GC-FID和GC-MS进行测定, 外标法定量。结果 GC-FID和GC-MS分别采用溶剂标准曲线和基质匹配标准曲线定量, 定量限分别为1.0 mg/kg和0.5 mg/kg, 线性范围分别为1~100 mg/kg和0.5~40.0 mg/kg, 添加回收率范围分别为88.9%~94.5%和91.2%~98.2%, 相对标准偏差范围分别为4.0%~6.4%和4.6%~7.3%; 两种方法检测结果基本一致, 相对偏差不超过2.4%。使用所建方法检测158批次中华蜜蜂蜂蜜和意大利蜜蜂蜂蜜, 结果仅在中华蜜蜂蜂蜜中检出17-三十五烯, 其含量范围为0.58~51.10 mg/kg。结论 本研究建立的GC-FID和GC-MS具有较高的灵敏度和准确度, 适用于蜂蜜中17-三十五烯的测定; 样品检测结果确证了17-三十五烯可以作为中华蜜蜂蜂蜜的特征标识物。

英文摘要:

      Objective To establish 2 kinds of methods for the determination of 17-pentatriacontene in honey by gas chromatography-flame ionization detection (GC-FID) and gas chromatography-mass spectrometry (GC-MS). Methods After dissolved in water, the sample was extracted with petroleum ether, purified on a florisil cartridge, separated by DB-5MS column (15 m×0.25 mm, 0.25 μm), and determined by GC-FID and GC-MS, then quantified by external standard method. Results The GC-FID and GC-MS were quantified using matrix-free standard curve and matrix-matched standard curve respectively, with limits of quantification of 1.0 mg/kg and 0.5 mg/kg, linear ranges of 1–100 mg/kg and 0.5–40.0 mg/kg, and recovery rates ranging from 88.9% to 94.5% and from 91.2% to 98.2%, respectively. The relative standard deviations were 4.0%–6.4% and 4.6%–7.3%, respectively. The results of the 2 kinds of methods were basically consistent, with a relative deviation of no more than 2.4%. The proposed methods were applied to 158 honey samples of Apis cerana honey and Apis mellifera honey, 17-pentatriacontene was only detected in Apis cerana honey, with a content range of 0.58–51.10 mg/kg. Conclusion The accuracy and precision of the GC-FID and GC-MS methods established in this study are both good, and the 2 kinds of methods can be applied to the determination of 17-pentatriacontene in honey. The results of real sample tested indicate that 17-pentatriacontene can be used as a characteristic marker for Apis cerana honey.