微波消解-电感耦合等离子体质谱法测定儿童爽身粉中微量硼  

Determination of trace boron in talcum powder for children by microwave digestion and ICP-MS

作　　者：郭珊珊 顾昉 肖紫芬 陈旭 卢端萍 Shanshan Guo;Fang Gu;Zifen Xiao;Xu Chen;Duanping Lu(Fujian Institute for Food and Drug Quality Control,Fuzhou,Fujian 350001,China;Fujian Environmental Impact Assessment Technology Center,Fuzhou,Fujian 350003,China)

机构地区：[1]福建省食品药品质量检验研究院,福建福州350001 [2]福建省环境影响评价技术中心,福建福州350003

出　　处：《日用化学工业》2022年第2期224-228,共5页China Surfactant Detergent & Cosmetics

摘　　要：利用微波消解前处理法,通过优化前处理和检测条件,针对儿童爽身粉(三岁以下)中不得检出硼酸和硼酸盐的规定,探索了一种电感耦合等离子体质谱(ICP-MS)法测定儿童爽身粉中的微量硼,实现了对硼元素在低质量浓度0~20 ng/mL范围内的准确定量。通过优化,最终选择HNO_(3)^(-)H_(2)O_(2)消解体系,消解程序为最终温度185℃,保持30 min,仪器分析模式为Nogas模式;同时考察了样品中共存离子的干扰情况。结果表明,Na^(+)、K^(+)、Ca^(2+)、Mg^(2+)、Fe^(2+)、Al^(3+)、Pb^(2+)、Zn^(2+)对硼的测定不产生干扰。该方法中硼的线性相关系数(r)为0.9999,检出限为0.02μg/g,定量限为0.07μg/g。在低、中、高三个质量浓度水平下的加标平均回收率为99.2%~101.4%。在阳性样品中,测定值的相对标准偏差RSD(n=6)为1.3%。实验结果表明,该方法准确、可靠、灵敏度高,适用于儿童爽身粉中硼酸和硼酸盐的测定,有助于加强对儿童爽身粉中硼酸和硼酸盐的风险管控。In this paper,according to the regulation that boric acid and borate should not be detected in talcum powder for children(under 3 years old),an inductively coupled plasma mass spectrometry(ICP-MS)method was explored to determine trace boron in children’s talcum powder.In exploratory stage,operation parameters of ICP-MS,microwave digestion pre-treatment,interference of coexisting ions were studied.By optimizing the microwave digestion system,HNO_(3)^(-)H_(2)O_(2) digestion solvent system was selected,and the temperature of the digestion procedure was raised to 185℃ for 30 minutes.In the process of optimizing instrument conditions,Nogas analysis mode was selected as the instrumental analysis mode,and yttrium(Y)was used as the internal standard element.Meanwhile,the test of interference with coexisting ions indicated that the common coexisting ions in talcum powder such as Na^(+),K^(+),Ca^(2+),Mg^(2+),Fe^(2+),Al^(3+),Pb^(2+),Zn^(2+) had no effects on the determination of boron.Under the best experimental conditions,the boron in the range of 0-20 ng/mL can be quantified accurately.The linear correlation coefficient(r)of the method is 0.9999.The detection limit of boron is as low as 0.02μg/g and the limit of quantitation of boron is 0.07μg/g.The recoveries of boron range from 99.2%to 101.4%at low,medium and high mass concentration spiked levels with 2,4,20 times of the quantitative concentration.The specific spiked concentrations are 25,50 and 250 ng and the relative standard deviations(RSDs)(n=3)of recovery experiments are between 2.2%and 5.4%.The RSD(n=6)of positive samples is 1.3%.The data above show that the method is accurate,reliable and sensitive.Applying the method to control quality of 30 batches of children’s talcum powder available in the market,trace boron are detected in 24 batches of the products.Boric acid is obtained through the conversion of the mass number of boron.The results are in accordance with the requirement of current standards.This method can be used for the accurate quantification o

关 键 词：微波消解 电感耦合等离子体质谱 爽身粉 硼元素 

分 类 号：TQ658[化学工程—精细化工]