顶空-气相色谱法测定天然胡萝卜素中的 溶剂残留量

Determination of organic solvent residues in natural carotenes by headspace-gas chromatography

中文关键词:  天然胡萝卜素  顶空-气相色谱法  N,N-二甲基乙酰胺  溶剂残留

英文关键词:natural carotenes  headspace-gas chromatography  N,N-dimethylacetamide  organic solvent residue

中文摘要:

      目的 建立顶空-气相色谱法测定天然胡萝卜素中的残留溶剂量。方法 样品经N,N-二甲基乙酰胺溶解, 经顶空进样, 采用HP-INNOWAX毛细管柱分离, 氢火焰离子化检测器检测, 以外标法定量。结果 在0~1000 mg/kg浓度范围内, 正己烷、丙酮、甲醇、异丙醇和乙醇5种残留溶剂呈良好的线性关系, 相关系数均大于0.995。各有机溶剂残留量的检出限为0.4~4.3 mg/kg; 在15、20和40 mg/kg 3个水平的加标量时, 加标回收率在85%~110%范围, 相对标准偏差均小于3%(n=6), 满足检测要求。结论 该方法操作简便、定量准确, 能满足天然胡萝卜素中残留溶剂量的检测需要。

英文摘要:

      Objective To establish a method for determination of organic solvent residue in natural carotenes by headspace-gas chromatography. Methods Samples were dissolved with N,N-dimethylacetamide, determined by gas chromatography with headspace sampling, separated by HP-INNOWAX column, and then detected by flame ionization detector with external standard method for quantification. Results Hexane, acetone, methanol, isopropyl alcohol and ethanol had good linear relationships in the range of 0~1000 mg/kg with correlation coefficients greater than 0.995, and the limits of detection were 0.4~4.3 mg/kg. The recoveries spiked at 3 levels of 15, 20 and 40 mg/kg were in the range of 85%~110% with RSDs less than 3% (n=6), which met the testing requirements. Conclusion The established method is simple and accurate, which can meet the requirements of determination of organic solvent residue in natural carotenes.