顶空-气相色谱法测定越橘提取物中的10种溶剂残留量

Determination of 10 kinds of solvents residues in bilberry extract by headspace-gas chromatography

中文关键词:  越橘提取物  溶剂残留  顶空-气相色谱法

英文关键词:bilberry extract  solvents residues  headspace-gas chromatography

中文摘要:

      目的 建立顶空-气相色谱法测定保健食品原料越橘提取物中正己烷、乙醇、苯、甲苯、对二甲苯、间二甲苯、邻二甲苯、苯乙烯、1,2-二乙基苯和二乙烯苯10种溶剂残留量的分析方法。方法 样品经顶空进样器95 ℃平衡30 min, 分流比为5:1 (V:V), 采用HP-FFAP石英毛细管柱(60 m×0.32 mm, 1.0 μm)分离, 程序升温, 氢火焰离子化检测器(flame ionization detector, FID)检测。结果 10种溶剂分离效果良好, 在其各自对应的浓度范围内线性关系良好(r≥0.9988); 方法检出限(limits of detection, LODs)为0.02~1.07 mg/kg; 3个添加水平下, 平均回收率为92.7%~116.4%, 相对标准偏差在0.2%~5.1% (n=3)之间。结论 该方法简便快速、结果可靠, 可用于保健食品原料越橘提取物的溶剂残留量的测定。

英文摘要:

      Objective To establish a method for the determination of 10 kinds of solvents residues in health food raw material bilberry extract, including n-hexane, ethanol, benzene, methylbenzene, p-xylene, m-xylene, o-xylene, styrene, 1,2-diethylbenzene and divinylbenzene by headspace-gas chromatography. Methods The samples were equilibrated at 95 ℃ for 30 min by headspace injector with a split ratio of 5:1 (V:V), and HP-FFAP quartz capillary column (60 m×0.32 mm, 1.0 μm) was used for separation, temperature programmed, hydrogen flame ionization detector (FID) was used for detection. Results The separation effects of 10 kinds of solvents were good, and the linear relationships were good in their corresponding concentration ranges (r≥0.9988); the limits of detection (LODs) were 0.02?1.07 mg/kg; the average recoveries for 10 kinds of solvents residues were in the range of 92.7%?116.4% at 3 spiked levels, and the relative standard deviations were 0.2% to 5.1% (n=3). Conclusion The method is simple, rapid and reliable, and can be used for the determination of solvents residues in health food raw material bilberry extract.