离子色谱-电感耦合等离子体质谱法测定饮用水中痕量无机锑(Ⅲ)  

Detection of trace inorganic antimony (Ⅲ) in water by ion chromatography-inductively coupled plasma mass spectrometry

作　　者：刘德晔[1] 姜新[1] LIU De-Ye;JIANG Xin(Jiangsu Provincial Center of Disease Control and Prevention,Nanjing,210009 China)

机构地区：[1]江苏省疾病预防控制中心

出　　处：《食品安全质量检测学报》2019年第23期8056-8061,共6页Journal of Food Safety and Quality

基　　金：江苏省“十三五”青年医学重点人才项目(QNRC2016540);江苏省医学重点学科(实验室)项目(ZDXKA2016008)~~

摘　　要：目的建立使用固相萃取(solid phase extraction, SPE)富集、在线氧化洗脱预处理,离子色谱-电感耦合等离子体质谱联用(ion chromatography-inductively coupled plasma mass spectrometry, IC-ICP-MS)测定饮用水中痕量三价无机锑(iSb(Ⅲ))的方法。方法水样中痕量iSb(Ⅲ)经过弱阳离子交换SPE柱富集后,依次使用甲醇、水净化,后使用1%H2O2+1%氨水混合溶液洗脱,洗脱液中iSb(Ⅲ)可全部转化为iSb(Ⅴ),IC-ICP-MS测定iSb(Ⅴ)浓度间接测得饮用水样中痕量iSb(Ⅲ)。水样中iSb(Ⅴ)不能被弱阳离子SPE富集,因此不干扰测定。结果富集倍率为10,方法在0.010~0.200μg/L范围内具有良好线性,相关系数r为0.996~0.998,检出限0.003~0.004μg/L,加标回收率94%~102%,日内相对标准偏差(RSD)1.7%~5.3%,日间精密度为0.6%。结论本方法稳定可靠,极低的检出限可用于饮用水中痕量甚至超痕量iSb(Ⅲ)的检测。Objective To establish a method for the determination of trace trivalent inorganic cerium [iSb(Ⅲ)] in drinking water by solid phase extraction enrichment(SPE), online oxidation elution pretreatment, and ion chromatography-inductively coupled plasma mass spectrometry(IC-ICP-MS). Methods Trace iSb(Ⅲ) was first enriched by a weak cationic exchange solid phase extraction(SPE) column, then purified by methanol and pure water. Finally, the enriched SPE column was eluted with 1% H2O2+1% NH3. The iSb(Ⅲ) in the eluent could be converted into iSb(Ⅴ) completely. Since the iSb(Ⅴ) could be easily detected by ion chromatography-inductively coupled plasma mass spectrometry(IC-ICP-MS) with shorter retention time and better peak shape, the iSb(Ⅲ) in water was measured indirectly. The iSb(Ⅴ) could not retain in a weak cationic exchange SPE column, so it brought no interfere with the method. Results When the enrichment factor was 10, the method had a satisfactory linearity with the curve ranging from 0.010 to 0.200 μg/L, and the linear coefficient r was 0.996-0.998. The LOD was of0.003-0.004 μg/L, and the recoveries were of 94%-102% with intra-day RSD of 1.7%-5.3% and inter-day RSD of 0.6%. Conclusion This method is stable and reliable, and the detection limit can be used for the detection of trace or even trace amounts of iSb(Ⅲ) in drinking water.

关 键 词：离子色谱-电感耦合等离子体质谱法 饮用水 三价无机锑 

分 类 号：O65[理学—分析化学]