【摘要】 目的:建立采用毛细管气相色谱测定肠内营养粉剂中碘的方法。方法:在酸性条件下过氧化氢将碘离子氧化为游离碘,游离碘与丁酮反应生成碘丁酮,再用正己烷萃取。采用气相色谱法,经RTX-225毛细管色谱柱分离,以电子捕获检测器检测。结果:碘浓度在0.002~0.020μg·mL-1范围内与衍生物峰面积的线性关系良好,r=0.9993(n=7);高、中、低浓度平均加样回收率分别为98.6%、100.1%和100.0%,RSD分别为0.55%、0.33%与0.48%;检测限为0.008 ng·mL-1,定量限为0.02 ng·mL-1。结论:经方法学验证,此方法灵敏度高,专属性好,结果准确,可用于肠内营养粉剂中微量碘的测定。更多还原

【Abstract】 Objective: To establish a capillary GC method for the assay of iodine in enteral nutritional powder.Methods: The iodine ion was oxidized to free iodine by hydrogen peroxide in acidic environment. Free iodine reacted with 2- butanone to produce iodobutanone,which was extracted with hexane after reaction. The assay was conducted by capillary gas chromatography on a RTX- 225 capillary column with an electron capture detector.Results: There was a good linear relationship between the area of the derivative and the concentration of iodine. The linear equation was Y = 1. 077 × 104X + 61. 30( r = 0. 9993) within the range of 0. 002- 0. 020 μg·mL- 1. The recoveries of high,medium and low concentrations were 98. 6%,100. 1% and 100. 0%( RSD = 0. 55%,0. 33% and0. 48%,n =3),respectively. The LOD was 0. 008 ng·mL- 1,and the LOQ was0.02 ng·mL- 1. Conclusion: The method verified by methodology is sensitive,reliable and accurate amd can be used for the assay of enteral nutritional powders.更多还原