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HS-GC法测定辣椒红色素中的有机溶剂残留

             

摘要

Object:A headspace gas chromatography was developed for simultaneous determination of five residual solvents (methanol,dichloromethane,ethanol,acetone and isopropanol) in paprika pigments.Method:Headspace sample gas chromatography was adopted.The equilibrium temperature was 80℃ and equilibrium time was 30min.The column temperature was maintained at 40℃ for 4min,then was raised to180℃ at the rate of 10℃/min for 4min,and then was raised again to 220℃ at the rate of 40℃/min for 3min.The solvent used was peanut oil: DMF (5: 5) and Agilent DB-WAX capillary column was adopted.Results:Good linear relationships were presented of the five residual solvents in their respective concentration ranges.The method provided accurate measurements (RSD < 5.0%),low detection limits (0.09 ~ 2.3 μg/g) and high recovery rates (98.0% ~ 102%,RSD < 5.0%,n=9).Conclusion:The method is simple and sensitive which provides reliable basis for the research of residual solvents in different kinds of Paprika Pigments.%目的:建立了同时测定辣椒红色素中甲醇、二氯甲烷、乙醇、丙酮和异丙醇5种残留溶剂的顶空气相色谱分析方法.方法:采用顶空进样法,平衡温度80℃,平衡时间30min,初始柱温温度为40℃保持4min,以10℃/min的速率升至180℃,保持4min,再以40℃/min的速率升至220℃,保持3min,以花生油:DMF(5:5)为溶剂,HP-MS为分析柱进行测定.结果:5种有机溶剂在各自的浓度范围内呈现良好的线性关系,方法精密度好(RSD<5.0%),检出限低0.09~2.3μg/g,样品加标回收率高98.0% ~ 102%,RSD<5.0% (n=9).结论:本方法简便、灵敏,为研究各种辣椒红色素中的残留溶剂提供了可靠的依据.

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