液相色谱-电感耦合等离子体质谱法测定生活饮用水中三价铬和六价铬含量的方法学验证与评价  

Validation of LC-ICP-MS method for the detection of trivalent and hexavalent chromium in drinking water

作　　者：袁鹏[1,2,3] 杨瑞春 张利锋[1,2,3] 李宗瑾 余根涛[4] 崔幸阳 马广周[4] 郭宴强[4] YUAN Peng;YANG Ruichun;ZHANG Lifeng;LI Zongjin;YU Gentao;CUI Xingyang;MA Guangzhou;GUO Yanqiang(Henan Center for Disease Control and Prevention,Zhengzhou,Henan 450016,China;Henan Key Laboratory of Food Safety Risk Monitoring and Assessment,Zhengzhou,Henan 450016,China;Henan Medical Key Laboratory of Foodborne Disease Etiological Traceability,Zhengzhou,Henan 450016,China;Pingdingshan Center for Disease Control and Prevention)

机构地区：[1]河南省疾病预防控制中心,河南郑州450016 [2]河南省食品安全风险监测与评价重点实验室,河南郑州450016 [3]河南省食源性疾病病原学溯源医学重点实验室,河南郑州450016 [4]平顶山市疾病预防控制中心

出　　处：《现代疾病预防控制》2023年第11期811-815,869,共6页MODERN DISEASE CONTROL AND PREVENTION

基　　金：河南省医学科技攻关计划联合共建项目(LHGT20220152);河南省重点研发与推广专项(科技攻关)项目(232102231040)。

摘　　要：目的 验证并评价《生活饮用水标准检验方法》GB/T 5750-2023修订过程中新增方法“液相色谱-电感耦合等离子体质谱法(LC-ICP-MS)测定生活饮用水及水源水中铬形态含量”的适用性、合理性和可操作性,为标准制定提供数据支撑,为采标实验室贯彻、执行该标准提供技术储备和参考。方法 根据标准研制初稿和资料查询意见拟定验证方案,对实验室试剂耗材、仪器状态、环境条件满足性予以确认,通过单标、混标进样建立、优化仪器条件,考察线性方程和线性范围,考察方法检出限、定量限,采集水源水、出厂水、末梢水和瓶装水考察实际样品测定的合理性与适用性,评价方法准确度和精密度,通过人员比对考察方法重现性和稳定性。结果 采用阴离子交换分析柱,60 mmol/L硝酸铵和0.6 mmol/L乙二胺四乙酸二钠(p H=7.0)为流动相,三价铬[Cr(Ⅲ)]与六价铬[Cr(Ⅵ)]分离良好,1.0~150.0μg/L范围内线性相关系数1.000,三价铬检出限0.222μg/L,定量限0.740μg/L;六价铬检出限为0.531μg/L,定量限为1.770μg/L。实际样品三价铬和六价铬测定相对标准偏差(RSD)<2.00%,加标回收率81.12%~112.12%,人员比对实测差<5.51%。结论 本方法样品处理简便合理,线性范围宽,灵敏度、准确度、精密度及重现性良好,适用于水源水、出厂水、末梢水、瓶装水三价铬、六价铬的准确测定,检出限充分满足目前相关限量标准要求。Objective To validate the applicability,rationality and operability of LC-ICP-MS method for the detection of trivalent and hexavalent chromium in drinking and source water,which was newly quoted in the amendment of GB/T 5750-2023(Standard Examination Methods for Drinking Water),and provide data support for the draft standard and technical reservation for accredited laboratories to evaluate and document the analytical performance prior to their first implementation and during ongoing operation.Methods The validation protocol was established based on the draft standard and document investigation;the laboratory satisfiability of reagents,consumables,instrument status and environmental conditions were confirmed.The instrument conditions were established and optimized through single and mixed standard sampling;the linear equation and linear range were investigated as well as the detection limit and quantitative limit of the method.The reasonableness and applicability of actual sample determination on source water,ex-factory water,peripheral water and bottled water were carried out to evaluate the accuracy and precision of the method;the reproducibility and stability of the method were examined by personnel comparison.Results Fine separation results of Cr(Ⅲ)and Cr(Ⅵ)were obtained with 60 mmol/L ammonium nitrate and 0.6 mmol/L disodium ethylenediamine tetraacetic acid(pH=7.0)as mobile phases.The linear correlation coefficient was 1.000 in the range of 1.0-150.0μg/L;the detection limit of Cr(Ⅲ)and Cr(Ⅵ)was 0.222μg/L and 0.531μg/L,respectively.The quantitation limit of Cr(Ⅲ)and Cr(Ⅵ)was 0.740μg/L and 1.770μg/L,respectively.For actual sample determination on Cr(Ⅲ)and Cr(Ⅵ),RSD was less than 2.00%,recoveries ranged from 81.12%to 112.12%,and the measured bias between different operators was less than 5.51%.Conclusions The method is simple and adaptable for sample processing with a wide linear range,good sensitivity,accuracy,precision and reproducibility,andis suitableforthe accurate determination ofCr(I)

关 键 词：LC-ICP-MS 生活饮用水 三价铬和六价铬 方法验证 

分 类 号：R123.1[医药卫生—环境卫生学]