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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。
Objective: To establish a method for determination of iodine in enteral nutrition powder by capillary gas chromatography. Methods: Under acidic conditions, hydrogen peroxide oxidizes iodide ions to free iodine, and free iodine and butanone react to form iodobutyl ketone, which is then extracted with n-hexane. Using gas chromatography, the RTX-225 capillary column separation, electron capture detector detection. Results: The linearity of peak area of iodine in the range of 0.002-0.020 μg · mL-1 was good, r = 0.9993 (n = 7). The average recoveries of high, medium and low concentrations were 98.6% 100.1% and 100.0% respectively. The RSDs were 0.55%, 0.33% and 0.48% respectively. The detection limit was 0.008 ng · mL-1 and the limit of quantification was 0.02 ng · mL-1. Conclusion: This method has high sensitivity, specificity and accuracy with method validation. It can be used for determination of trace iodine in enteral nutrition powder.