饮料中乙酰磺胺酸钾的高效液相色谱测定法.pdfVIP

1520 职业与健康 2008年8月第24卷第l5期 Occup and Heath Vo1．24 No．15 Aug 2008 饮料中乙酰磺胺酸钾的 【实验 ·监测与检验】 高效液相色谱测定法 High Performance Liquid Chromatography in the Determination of Acetylsulfame K in the Beverages 卢丽明，黄诚，周日东 LU Li—ming，HUANG Cheng，ZHOU Ri—dong 摘要 目的 建立高效液相色谱测定饮料中乙酰磺胺酸钾的方法。方法 用流动相CH OH／0．02 mol／L NH Ac替代I 标 法CH OH／CH CN／0．02 mol／L(NH ) SO ／10％H SO ，样品处理后经高效液相反相分离后，采用色谱保留时间定性，峰高或 峰面积定量进行测定，同时对方法进行回收率、精密度、线性关系验证试验以及2种方法的比对试验。结果 在选定的色谱 条件下，用c OH／0．02 mol／L NH Ac作流动相，标准曲线的线性关系良好，其相关系数值为0．9999；精密度试验结果，相 对标准偏差为0．15％～0．64％(n=6)；样品加标回收率为98．1％～99．8％；TY法的最低检出浓度为0．43 ml；用2种不 同流动相进行方法比对试验，结果差异无统计学意义(P0．01)。结论 该方法操作简单、避免了使用有较大毒性的 CH CN，而且方法精密度、准确度均能满足实验要求，结果可靠。 关键词 高效液相色谱法；饮料；乙酰磺胺酸钾 中国图书资料分类号：R115 文献标识码：B 文章编号：1004—1257(2008)15—1520—02 Subject High Performance Liquid Chromatography in the Determination of Acetylsulfame K in the Beverages Authors LU Li—ming，HUANG Cheng，ZHOU Ri—dong(Zhongshan Center r Disease Control and Prevention，Guangdong， 528403，China) Abstract [Objective]To establish HPLC method for the determination of acetylsulfame K in the beverages．[Methods]Fluid chromatography CH3OH／0．02 mol／L NH4AC was applied to take place of the international method CH3OH／CH3CN／0．02 mol／L (NH4)2SO4／10％H2SO4；the samples were retained for quantification with chromatography after being separated with high perform— ance liquid；determination was made on the peak height or the peak area，meanwhile，test was made on the recovery rate，precision and linear correlations；comparison was made between the two methods．[Results]Under the condition of the chosen chromatography using CH3OH／0．02 mol／L NH4AC as the fluld，the standard curve showed good linear correlations with the coefficient of 0．9999； the precision test showed thatRSDwas 0．15％～0．64％(n=6)；the labeled recovery rate ofthe samples was 98．1～99．8％；the LOD 0．43 ml；no significant dif