四甲基氢氧化铵提取-高分辨电感耦合等离子体质谱法测定头发中碘  

Determination of iodine in hair by tetramethylammonium hydroxide extraction-high resolution inductively coupled plasma mass spectrometry

作　　者：李如燕 赵越 胡萍 张如莹 LI Ruyan;ZHAO Yue;HU Ping;ZHANG Ruying(Geological Survey of Jiangsu Province,Nanjing 210018,China)

机构地区：[1]江苏省地质调查研究院,南京210018

出　　处：《化学分析计量》2025年第2期72-76,共5页Chemical Analysis And Meterage

摘　　要：建立了四甲基氢氧化铵(TMAH)提取-高分辨电感耦合等离子体质谱法测定头发中碘含量。取干燥剪碎后的头发样品0.1 g,置于耐高温的50 m L塑料离心管中,加入5 m L质量分数为2%的TMAH溶液,旋紧盖子,涡旋1min后,于恒温干燥箱中(85±5)℃提取3 h。冷却后用水定容至标线,离心,取上层清液,用0.45μm滤膜过滤,以高分辨电感耦合等离子体质谱仪测定滤液中碘含量。以铑作为内标元素校正仪器信号漂移,选择合适的分辨率,有效消除基体效应及多原子离子产生的质谱干扰。碘的质量浓度在0~20.0 ng/m L内与对应的质谱信号强度线性相关,检出限为0.005 58 mg/kg。该方法用于国家一级标准物质和实际样品的分析,测定值的相对误差为1.25%,测定值的相对标准偏差为3.55%~4.59%(n=12),加标回收率为97.3%~104%。该方法简单、准确,适用于头发样品中碘含量的测定。A method for the determination of iodine in hair by tetramethylammonium hydroxide(TMAH)extraction-high resolution inductively coupled plasma mass spectrometry was established.0.1 g of dried and chopped hair sample was put into a 50 mL plastic centrifuge tube with high temperature resistance,5 mL of TMAH solution with mass fraction of 2%was added,the lid was vortexed for 1 min,and then extracted for 3 h at(85±5)℃in a constant temperature drying oven.After cooling,the sample was diluted with water to scale.After centrifugation,the supernatant was filtered with 0.45μm filter membrane,and the content of iodine in the filtrate was determined by high resolution inductively coupled plasma mass spectrometry.Rhodium was used as the internal standard element to correct the signal drift of the instrument,and the appropriate resolution was selected to effectively eliminate the matrix effect and the mass spectrometry interference caused by polyatomic ions.The mass concentration of iodine in the range of 0-20.0 ng/mL showed a linear relationship with the corresponding mass spectrometry signal intensity,and the detection limit was 0.00558 mg/kg.The method was applied to the analysis of national standard reference materials and actual samples.The relative error of the measured value was 1.25%,the relative standard deviation of the measured value was 3.55%-4.59%(n=12),and the recovery rate was 97.3%-104%.The method is simple,accurate and suitable for the determination of iodine content in hair samples.

关 键 词：四甲基氢氧化铵 高分辨电感耦合等离子体质谱法 头发 碘 

分 类 号：O657.6[理学—分析化学]