摘要
目的优化高效液相色谱-质谱测定尿中苯巯基尿酸(SPMA)方法中的萃取和定量方法。方法尿液采用体积分数50.0%的硫酸进行水解;水解液采用固相萃取柱进行净化,经C18色谱柱分离,串联质谱检测。以同位素标记的SPMA作为内标,以内标工作曲线法定量。结果SPMA的线性范围为0.50~50.00μg/L,相关系数为0.9998;方法的检出限和定量限分别为0.05和0.17μg/L;加标回收率为97.0%~102.0%,批内相对标准偏差(RSD)为0.6%~1.0%,批间RSD为1.7%~6.5%。采用本方法检测,职业性苯接触组人群尿中SPMA质量浓度高于无职业接触组(中位数:2.81 vs 0.28μg/g肌酐,P<0.05)。结论与国家标准方法比较,本方法采用固相萃取和内标法定量,改进后的方法有利于消除基质效应,准确度和精密度好,适用于尿中SPMA的测定。
Objective To optimize the extraction and quantification methods for the determination of S-phenylmercapturic acid(SPMA)in urine with performance liquid chromatography-mass spectrometry.Methods The urine was hydrolyzed with 50.0%sulfuric acid.The hydrolysate was purified by solid phase extraction column.Purified samples were separated by C18 chromatographic column and detected by tandem mass spectrometry.The isotope labeled SPMA was used as the internal standard.The internal standard curve was used for quantification.Results The linear range of SPMA was 0.50-50.00μg/L with the correlation coefficient of 0.9998.The detection limit and the lower limit of quantification were 0.05 and 0.17μg/L,respectively.The recovery rate was 97.0%-102.0%.The within-run and between-run relative standard deviation were 0.6%-1.0%and 1.7%-6.5%,respectively.The mass concentration of urinary SPMA in the occupational benzene exposure group was higher than the non-occupational benzene exposure group by this method(median:2.81 vs 0.28μg/g creatinine,P<0.05).Conclusion Compared to the national standard method,this optimized method of solid phase extraction and internal standard for quantification eliminates the matrix effect.This method is accurate and precise,and is suitable for the determination of SPMA acid in urine.
作者
崔师伟
周晓滢
邢彩虹
闫慧芳
CUI Shi-wei;ZHOU Xiao-ying;XING Cai-hong;YAN Hui-fang(National Institute of Occupational Health and Poison Control,Chinese Center for Disease Control and Prevention,Beijing 100050,China)
出处
《中国职业医学》
CAS
北大核心
2022年第6期692-696,共5页
China Occupational Medicine
基金
国家自然科学基金(81641009)
关键词
苯巯基尿酸
固相萃取
同位素
内标
高效液相色谱
质谱
尿
S-phenylmercapturic acid
Solid phase extraction
Isotope
Internal standard
Performance liquid chromatography
Mass spectrometry
Urine
作者简介
崔师伟(1985—),男,分析化学硕士,副研究员,主要从事理化检测工作
