电感耦合等离子体质谱法测定化妆品中汞元素的含量  

Determination of Mercury Element in Cosmetics by Inductively Coupled Plasma Mass Spectrometry

作　　者：胡丹 石瑞瑞 汪淼峰 金梦芸 李长于 叶涛 HU Dan;SHI Ruirui;WANG Miaofeng;JIN Mengyun;LI Changyu;YE Tao(Zhejiang Fang Yuan Test Group Co.,Ltd.,Hangzhou 310018,China)

机构地区：[1]浙江方圆检测集团股份有限公司,杭州310018

出　　处：《理化检验（化学分册）》2024年第11期1119-1123,共5页Physical Testing and Chemical Analysis(Part B:Chemical Analysis)

基　　金：浙江省市场监督管理局科研项目(ZC2021A032)。

摘　　要：针对电感耦合等离子体质谱法(ICP-MS)测定汞元素时存在汞记忆效应严重,且消除时前处理过程复杂的问题,提出了此项研究。取样品0.5000 g置于聚四氟乙烯消解罐中,加入5 m L硝酸和1 m L 30%(质量分数)过氧化氢溶液,置于100℃恒温消解仪中加热30 min,冷却,将消解罐密封置于微波消解仪中,消解后冷却,打开消解罐,置于100℃恒温消解仪中15 min,将消解溶液转移至25 m L容量瓶中,用水洗涤消解罐数次,清洗液与消解溶液合并,用水定容至25 m L,与清洗试剂[2 mg·L^(-1)金元素标准使用液或2%(质量分数,下同)L-半胱氨酸溶液]配制的20μg·L^(-1)186Re内标溶液在线混匀后,采用ICP-MS进行测定。结果表明,清洗试剂可消除0.5~5μg·L^(-1)汞元素标准溶液的汞记忆效应,对下一个样品的测定结果不产生影响。汞元素的质量浓度在0.5~5μg·L^(-1)内与所对应的信号强度与内标元素信号强度比呈线性关系,采用2 mg·L^(-1)金元素标准使用液配制内标溶液时,检出限(3s)为0.0010 mg·kg^(-1),采用2%L-半胱氨酸溶液配制内标溶液时,检出限(3s)为0.0012 mg·kg^(-1)。按照标准加入法进行回收试验,回收率为90.2%~104%,测定值的相对标准偏差(n=6)均小于9.0%。方法用于3种市售化妆品分析,使用2种清洗试剂配制的内标溶液得到的检出量一致,为0.0080~0.13 mg·kg^(-1)。In view of the serious mercury memory effect and the complicated elimination pretreatment process in determination of mercury element by inductively coupled plasma mass spectrometry(ICP-MS),this study was proposed.0.5000 g of sample was taken and placed in a polytetrafluoroethylene digestion tank,and 5 mL of nitric acid and 1 mL of 30%(mass fraction)hydrogen peroxide solution were added.The mixture was heated at 100℃for 30 min in a constant temperature digestion instrument and cooled.The digestion tank was sealed and placed in a microwave digestion instrument.After digestion,the digestion tank was cooled and opened,and placed at 100℃for 15 min in a constant temperature digestion instrument.The digestion solution was taken and placed in a 25 mL-volumetric flask,and the digestion tank was washed several times with water.The washing solutions were combined with the digestion solution,and the solution was made up to 25 mL with water.The 20μg·L^(−1)186Re internal standard solution,which was prepared with cleaning reagents[2 mg·L^(−1) gold element standard solution or 2%(mass fraction,the same below)L-cysteine solution],was mixed online with the sample solution for determination by ICP-MS.As shown by the results,the cleaning reagents could eliminate the mercury memory effect of 0.5−5μg·L^(−1) mercury element standard solution,without affecting the determination of the next sample.Linear relationships between the ratios of the corresponding signal intensity to the internal standard signal intensity and mass concentrations of mercury element were found in the range of 0.5−5μg·L^(−1),with detection limit(3s)of 0.0010 mg·kg^(−1) by using 2 mg·L^(−1) gold element standard solution to prepare an internal standard solution,and detection limit(3s)of 0.0012 mg·kg^(−1) by using 2%L-cysteine solution to prepare an internal standard solution.Test for recovery was made by the standard addition method,giving results in the range of 90.2%−104%,with RSDs(n=6)of the determined values less than 9.0%.Thi

关 键 词：电感耦合等离子体质谱法(ICP-MS) 化妆品 汞记忆效应 金 L-半胱氨酸 

分 类 号：O657.63[理学—分析化学]