首页|UPLC-MS/MS同位素内标法同时测定尿液中高氯酸盐、硫氰酸盐、硝酸盐含量

UPLC-MS/MS同位素内标法同时测定尿液中高氯酸盐、硫氰酸盐、硝酸盐含量

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目的 建立高效液相色谱串联质谱法同时检测尿液中高氯酸盐、硫氰酸盐和硝酸盐的分析方法.方法 取人尿样品并加入高氯酸盐、硫氰酸盐和硝酸盐混合内标,充分涡旋振荡和高速离心后,取上清液经色谱分析柱分离,液相色谱串联质谱测定高氯酸盐、硫氰酸盐和硝酸盐,内标法进行定量.结果 高氯酸盐、硫氰酸盐和硝酸盐分别在 1~200 μg/L、3~600 μg/L和 1~200 mg/L浓度范围内具有较好的线性关系,决定系数 R2 分别为 0.999、0.999 和 0.995.高氯酸盐、硫氰酸盐和硝酸盐检出限分别为 0.3 μg/L、1.0 μg/L 和 0.3 mg/L,平均加标回收率分别为 95.8%~101.7%、98.3%~104.6%和 99.3%~100.4%.结论 本方法具有样品前处理步骤简单,上机检测耗时短、待测物质的专属性高、稳定性好、灵敏度高的优点,可以满足批量人尿样本中高氯酸盐、硫氰酸盐和硝酸盐含量检测的需求.
Simultaneous determination of perchlorate,thiocyanate,and nitrate contents in urine by UPLC-MS/MS with isotope internal standards
Objective To establish ultra-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)for sim-ultaneous determination of perchlorate,thiocyanate,and nitrate in urine.Methods Urine samples were mixed with a mixture of inter-nal standards of perchlorate,thiocyanate,and nitrate for swirling and high-speed centrifugation,and the supernatants were separated through a column.The contents of perchlorate,thiocyanate,and nitrate were determined by HPLC-MS/MS with the internal standard method.Results Perchlorate,thiocyanate,and nitrate showed good linearity within the concentration ranges of 1-200 μg/L,3-600 μg/L,and 1-200 mg/L,respectively,with correlation coefficients of determination(R2)of 0.999,0.999,and 0.995,respec-tively.The detection limits of perchlorate,thiocyanate,and nitrate were 0.3 μg/L,1.0 μg/L and 0.3 mg/L,with the recovery rates of 95.8%-101.7%,98.4%-104.6%,and 99.3%-100.4%,respectively.Conclusion This method has the advantages of simple sample pretreatment,short detection time,high specificity for substances to be measured,good stability,and high sensitivity,which can meet the requirements of determining perchlorate,thiocyanate,and nitrate for large quantities of human urine samples.

liquid chromatography-mass spectrometryperchloratenitratethiocyanate

于帅、周旭东、周婧、付若楠、陆一凡、王琛琛、杨玉玲、潘凯

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博尔塔拉蒙古自治州疾病预防控制中心,博尔塔拉蒙古自治州 833400

新疆医科大学公共卫生学院

新疆维吾尔自治区疾病预防控制中心

液相色谱串联质谱 高氯酸盐 硝酸盐 硫氰酸盐

国家自然科学基金项目国家卫生健康委病因流行病学重点实验室(哈尔滨医科大学)开放课题

82260648NH-CKLEE20230906

2024

环境卫生学杂志
中国疾病预防控制中心

环境卫生学杂志

CSTPCD
影响因子:0.735
ISSN:2095-1906
年,卷(期):2024.14(10)
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