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  

Simultaneous determination of perchlorate,thiocyanate,and nitrate contents in urine by UPLC-MS/MS with isotope internal standards

作　　者：于帅 周旭东 周婧 付若楠 陆一凡 王琛琛[3] 杨玉玲 潘凯[3] YU Shuai;ZHOU Xu-dong;ZHOU Jing;FU Ruo-nan;LU Yi-fan;WANG Chen-chen;YANG Yu-ling;PAN Kai(Center for Disease Control and Prevention of Bortala Mongol Autonomous Prefecture,Bortala Mongol Autonomous Prefecture 833400,China;School of Public Health,Xinjiang Medical University;Xinjiang Uygur Autonomous Region Center for Disease Control and Prevention)

机构地区：[1]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 [2]新疆医科大学公共卫生学院 [3]新疆维吾尔自治区疾病预防控制中心

出　　处：《环境卫生学杂志》2024年第10期860-865,876,共7页JOURNAL OF ENVIRONMENTAL HYGIENE

基　　金：国家自然科学基金项目(82260648);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(NHCKLEE20230906)。

摘　　要：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1~200μg/L、3~600μg/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0.3μg/L、1.0μg/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。Objective To establish ultra-performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)for simultaneous determination of perchlorate,thiocyanate,and nitrate in urine.Methods Urine samples were mixed with a mixture of internal 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 1-200μg/L,3-600μg/L,and 1-200 mg/L,respectively,with correlation coefficients of determination(R2)of 0.999,0.999,and 0.995,respectively.The detection limits of perchlorate,thiocyanate,and nitrate were 0.3μg/L,1.0μg/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.

关 键 词：液相色谱串联质谱 高氯酸盐 硝酸盐 硫氰酸盐 

分 类 号：O657.6[理学—分析化学] R115[理学—化学]