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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。
Objective To establish a headspace-gas chromatographic method for the determination of residual solvents in natural carotenoids. Methods The sample was dissolved in N, N-dimethylacetamide, injected through the headspace, separated by HP-INNOWAX capillary column, detected by flame ionization detector and quantified by external standard method. Results In the range of 0-1000 mg / kg, the five residual solvents of n-hexane, acetone, methanol, isopropanol and ethanol showed a good linear relationship with the correlation coefficients greater than 0.995. The detection limit of each organic solvent was 0.4 ~ 4.3 mg / kg. The spike recoveries ranged from 85% to 110% at the spiked levels of 15, 20 and 40 mg / kg. The relative standard deviations Less than 3% (n = 6), to meet the testing requirements. Conclusion The method is simple, accurate and can meet the detection needs of the residual solvent in natural carotene.