目的 建立简便快速消解奶粉样品,实现其总碘含量测定的方法。 方法 用高氯酸、氯酸钾混合湿法消解样品溶液2小时,用砷铈催化分光光度法测定其碘含量。由吸光度值与碘浓度的对应关系,计算出样品中碘的含量。结果 检测范围0~100 μg/L,标准曲线相关系数为-0.999 6~-0.999 9;精密度:测定奶溶液样品中碘含量为20.11 μg/L、60.45 μg/L和86.55 μg/L时,变异系数(CV)分别为2.54%、1.85%和1.58%;准确度:对低、中、高3种不同浓度碘含量的奶粉溶液加标回收率分别为98.90%、101.02%和99.66%(n=6),平均回收率为99.86%。结论 本方法适合应用于奶粉中总碘的含量测定。
Abstract
Objective To establish a simple and rapid method for the determination of iodine content in milk powder samples. Methods The content of iodine was determined by the method of perchloric acid and potassium perchlorate in 2 hours, and the iodine content of the sample was determined by arsenic cerium catalytic spectrophotometry. According to the corresponding relationship between the absorbance value and the iodine concentration, the content of iodine in the sample was calculated. Results When the detection range was 0-100 μg/L, the correlation coefficient of the standard curve was between -0.999 6 and -0.999 9. Precision: when the determination of iodine content in milk sample solution were 20.11 μg/L, 60.45 μg/L and 86.55 μg/L, the coefficients of variation (CV) were 2.54%, 1.85% and 1.58% respectively. Accuracy: the recovery rate of the 3 different concentration iodine contents in milk powder water solution were 98.90%, 101.02% and 99.66% (n=6), and the average recovery rate was 99.86%. Conclusion The method is suitable for the determination of total iodine content in milk powder.
关键词
湿法消解 /
奶粉 /
砷铈催化 /
分光光度法 /
碘
Key words
Wet digestion /
Milk powder /
Arsenic cerium catalysis /
Spectrophotometry /
Iodine
{{custom_sec.title}}
{{custom_sec.title}}
{{custom_sec.content}}
参考文献
[1] 刘列钧, 李秀维, 李淑华, 等. 碱灰化砷铈催化分光光度法测定鲜奶及奶粉中碘含量[J].中国地方病防治杂志, 2006, 21(2):79-81.
[2] 高元, 刘悦, 管蓉, 等. 砷铈催化比色法测定奶粉中微量碘的研究[J].职业与健康, 2002, 18(5): 38-39.
[3] 刘中文, 孙咏梅. 气相色谱法测定奶粉中的碘[J].解放军预防医学杂志,2002, 20(1):31-32.
[4] 樊祥, 王敏, 陈迪, 等. 电感耦合等离子体质谱法分析婴幼儿配方奶粉中碘[J].分析科学学报,2014, 30(6):919-922.
[5] Picoloto RS,Doneda M,Flores ELM,et al. Simultaneous determination of bromine and iodine in milk powder for adult and infant nutrition by plasma based techniques after digestion using microwave-induced combustion[J].Spectroscopy,2015, 107(1):86-92.
[6] Huynh D,Zhou SJ,Gibson R, et al. Validation of an optimized method for the determination of iodine in human breast milk by inductively coupled plasma mass spectrometry(ICP-MS) after tetramethylammonium hydroxide extraction[J].J Trace Elem Med Biol, 2015, 29:75-82.
[7] 焦霞, 朱富强, 杨兰玲,等. 离子色谱紫外检测器联用技术同时分离测定乳制品中的I-和SCN-[J].分析化学,2009, 37(A02):265-266.
[8] 奉夏平, 叶祥平, 姚春燕,等. 灰化气相色谱/质谱法测定奶粉中碘的研究[J].分析科学学报,2009, 25(2);241-243.
[9] 柴成文, 刘克纳, 牟世芬. 安培检测-离子色谱法测定乳品中的微量碘[J].色谱, 2001, 19(1):94-96.
[10] 焦霞, 鲁联合, 盖学武. 离子色谱紫外检测器联用技术同时分析测定乳制品中的碘离子和硫氰酸根[J].化学分析计量,2010, 19(1):33-35.
[11] 张亚平, 阎玉芹, 刘列钧,等. 尿中碘的过硫酸铵消化-低砷量砷铈催化分光光度测定方法[J].中华地方病学杂志, 2013, 32(1):95-100.
[12] 中华人民共和国卫生行业标准. 尿中碘的砷铈催化分光光度测定法(WS/T 106-2006)[S].北京:人民卫生标准出版社, 2006.
[13] 刘中文,孙咏梅. 气相色谱法测定奶粉中的碘[J].解放军预防医学杂志, 2002, 20(1):31-32.
[14] 王娟, 孙军, 张朝燕, 等. 离子色谱法测定奶粉中阴、阳离子[J].食品质量安全与检测, 2007, 10:24-25,29.
[15] 刘丽萍, 吕超, 谭玲, 等. 电感耦合等离子体质谱法测定乳制品中碘含量的方法研究[J].2010, 31(3):138-142.
[16] 徐敏, 郝义. 催化动力学光度法测定痕量的碘[J].化学与黏合, 2007, 29(3):223-225.
[17] 卫生部. 研制生物样品监测检验方法指南(WS/T 68-1996)[S].北京:中国标准出版社,1996.