摘要
建立了顶空气相色谱法(HSGC)同时测定三氯蔗糖中甲醇、乙酸乙酯和乙酸丁酯残留量的分析方法。用Angilent Innowax毛细柱,程序升温,FID检测器,以保留时间定性,外标法定量,探讨了盐溶液、相比、平衡温度、平衡时间和振荡幅度等因素对测定结果的影响。结果表明,以100 g/L NaCl溶液为溶解液,取1mL溶液于20 mL顶空瓶中,平衡温度为80℃,平衡时间为15 min,振荡幅度低的条件下,该方法线性关系良好,3种物质线性方程的相关系数r在0.9999~1之间;方法精密度RSD(n=6)小于2.0%。三氯蔗糖样品的加标平均回收率均在95%以上。
A method for the determination of the residual solvents(methanol,ethyl acetate and butyl acetate)in sucralose by headspace gas chromatography(HSGC) was developed.A capillary column(Innowax) and flame ionization detector(FID) were used in the GC analysis.The species identification and quantification were performed by retention time based on the external standard samples.The effects of the salting-out,phase ratio,temperature,equilibration time,and agitation on the quantification of species were investigated.The results showed that using 1 mL of NaCl solution(100 g/L) as the sample matrix at a temperature of 80 ℃for 15-min equilibration and a low agitation,the contents of methanol,ethyl acetate and butyl acetate can be accurately quantified,in which the linear GC response ranges for these species were 3.72～464.5,0.48～60.5,and 0.32～39.25μg/mL,respectively,with the regression coefficients between 0.9999 and 1.000.The relative standard deviations(RSD) in the quantification of methanol,ethyl acetate and butyl acetate were 1.4%,1.0% and 1.1%,respectively.The average recoveries from sucralose samples were better than 95%.The method is simple,rapid,sensitive,accurate and safe.
出处
《分析试验室》
CAS
CSCD
北大核心
2010年第10期64-67,共4页
Chinese Journal of Analysis Laboratory
基金
河北师范大学(L2009Y12)项目资助
关键词
顶空气相色谱
三氯蔗糖
有机溶剂残留
Headspace gas chromatography(HSGC)
Sucralose
Solvent residues
