电感耦合等离子体质谱-标准加入法测定婴幼儿辅食米粉中锡含量  

Determination of Tin in Infant Supplementary Food Rice Powder Using Inductively Coupled Plasma Mass Spectrometry with Standard Addition Method

作　　者：张世龙 蔡玮 赵博[2] 陈欢欢 逯海[2] 李潇[2] ZHANG Shilong;CAI Wei;ZHAO Bo;CHEN Huanhuan;LU Hai;LI Xiao(Jiangxi General Institute of Testing and Certification Donghua Institute of Metrology and Testing,Nanchang 330031,China;National Institute of Metrology,Beijing 100029,China)

机构地区：[1]江西省检验检测认证总院东华计量测试研究院,南昌330031 [2]中国计量科学研究院,北京100029

出　　处：《计量科学与技术》2023年第12期20-26,共7页Metrology Science and Technology

摘　　要：采用外标法和标准加入法分别对婴幼儿辅食米粉中锡含量进行定量分析,研究了锡含量结果在预消解加入不同酸及复杂基质时所受的影响,建立了电感耦合等离子体质谱法(inductively coupled plasma-mass spectrometry,ICP-MS)准确测定婴幼儿辅食米粉中锡含量的测定方法,分析了婴幼儿辅食米粉测定过程的不确定度来源,评定了各不确定度分量并合成得到方法的扩展不确定度。分析结果表明,采用硝酸预反应后补加盐酸进行微波消解前处理,标准加入法分析锡的相关线性(r 2)在0.9998以上,方法检出限为0.02 mg/kg,对有证标准物质的测量偏差为+1.2%。通过对婴幼儿辅食米粉中锡含量进行测定,加标回收率为100.5%~104.5%,当锡含量为1.31 mg/kg时,扩展不确定度为0.04 mg/kg(k=2)。相较于外标法,标准加入法适用于婴幼儿辅食米粉基体标准物质研制过程中锡含量的定值,方法准确可靠。Quantitative analysis of tin content in infant supplementary food rice powder was conducted using external standard and standard addition methods.The study investigated the effects of different acids added during pre-digestion and complex matrices on the tin content results.An accurate method for determining tin content in infant supplementary food rice powder was established using Inductively Coupled Plasma-Mass Spectrometry(ICP-MS).The study analyzed the sources of uncertainty in the determination process of infant supplementary food rice powder,evaluated each component of uncertainty,and calculated the method's expanded uncertainty.The analysis showed that pre-digestion with nitric acid followed by the addition of hydrochloric acid before microwave digestion,and the standard addition method for tin analysis resulted in a correlation coefficient(r2)above 0.9998.The method detection limit was 0.02 mg/kg,and the measurement deviation for certified reference material was+1.2%.When tin content was measured at 1.31 mg/kg,the expanded uncertainty was 0.04 mg/kg with a coverage factor of k=2.The standard addition method was suitable for determining tin content in infant supplementary food rice powder,proving to be more accurate and reliable.

关 键 词：计量学 电感耦合等离子体质谱法 标准加入法 基质效应 锡 婴幼儿辅食米粉 

分 类 号：TB99[一般工业技术—计量学]