顶空气相色谱法优化奶粉中碘的检测  

Optimizing the detection of iodine in milk powder by headspace-gas chromatography

作　　者：蔡德玲[1] 梁玉英[1] 范稚莉[1] CAI De-ling;LIANG Yu-ying;FAN Zhi-li(Inspection Technical Center of Zhuhai Entry-Exit Inspection and Quarantine Bureau,Zhuhai 519000,China)

机构地区：[1]珠海出入境检验检疫局技术中心,广东珠海519000

出　　处：《化学工程师》2018年第7期31-34,共4页Chemical Engineer

基　　金：珠海出入境检验检疫局科研项目(No.ZH2016-14)

摘　　要：建立了基于正交实验的顶空气相色谱法优化奶粉中碘的检测。将奶粉中碘和丁酮衍生成碘丁酮后,抽取顶空瓶上层气体,经HP-5毛细管色谱柱分离,气相色谱电子捕获检测器检测。该方法在线性范围为1~12μg内呈现较好的相关性,其相关系数(r^2)为0.9997,其方法检出限为0.02 mg·kg^(-1)。样品加标实验回收率在89.7%~101.4%之间,相对标准偏差为4.7%。此方法具有快速、简便、灵敏度高、重线性好、试剂用量少等特点,为奶粉中碘的快速检测提供技术支持。A method based on the orthogonal experiment was established for the determination of iodine in milk powder by headspace-Gas chromatography. After derivazation of iodine to iodine butanone, the headspaee gas was extracted for separation by HP-5 capillary column and detected with electronic capture detector （ECD）. The method showed a good linearity in the range of 1-12μg with correlation coefficient （r2） larger than 0.999, and the limit of detection was 0.02 mg·kg-1 The recoveries of method precision were from 89.7% to 101.4%, and the RSD was 4.7%. The method is quick, simple, sensitive, reproductive, economical and suitable for the rapid determination of iodine in milk powder.

关 键 词：碘 奶粉 正交实验 气相色谱法 顶空进样 

分 类 号：O65[理学—分析化学]