UPLC-MS/MS法测定工作场所空气中苯胺和对硝基苯胺  

Determination of aniline and p-nitroaniline in workplace air by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：陈祝军[1] 秦园 吴建兵[1] 钱志荣[1] 吴梅[1] 王露[2] CHEN Zhujun;QIN Yuan;WU Jianbing;QIAN Zhirong;WU Mei;WANG Lu(Department of Physiochemical Inspection,Zhangjiagang Center for Disease Control and Prevention,Suzhou,Jiangsu 215600,China;不详)

机构地区：[1]张家港市疾病预防控制中心理化检验科,江苏苏州215600 [2]淮安市疾病预防控制中心

出　　处：《医学动物防制》2024年第10期999-1002,共4页Journal of Medical Pest Control

基　　金：江苏省预防医学科研课题(Ym2023022);张家港市科技支撑计划(社会发展)(ZKS1921)。

摘　　要：目的探索超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)法测定工作场所空气中苯胺和对硝基苯胺的方法。方法工作场所空气中苯胺和对硝基苯胺经硅胶管采集,甲醇解吸后直接进样,以甲醇∶水(70∶30,V/V)为流动相等度洗脱,经C_(18)色谱柱(2.1mm×50.0mm,1.7μm,美国Waters公司)分离,采用电喷雾离子源正离子、多反应检测模式检测。采用t检验对工作场所空气中的苯胺和对硝基苯胺含量进行比较。结果在最佳分析条件下,苯胺和对硝基苯胺的检出限分别为0.5μg/ml和0.1μg/ml;苯胺(0~50.0μg/ml)、对硝基苯胺(0~10.0μg/ml)线性范围内的线性关系良好,相关系数(r)均>0.999;样品解吸效率为96.40%~97.88%;加标回收率为96.50%~99.17%;相对标准偏差为2.37%~4.36%(n=6)。质谱法和国标法对空气中苯胺和对硝基苯胺的检测结果差异无统计学意义(F=0.007、0.065,t=0.084、0.256,P>0.05)。结论该方法操作简便,目标物分离度高、重现性好、灵敏度高,可以作为工作场所空气中苯胺、对硝基苯胺的日常检测方法。Objective To explore ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for determination of aniline and p-nitroaniline in workplace air.Methods The aniline and p-nitroaniline in workplace air were sampled by silica gel tube,desorbed by methanol and injected directly into the sample.Methanol∶water(70∶30,V/V)was used as the mobile phase isocratic elution.It was separated on a C_(18)column(2.1mm×50.0mm,1.7μm,Waters Corporation,USA)and detected by an electrospray ionization source in positive ion,multi-reaction detection mode.The t-test was used to compare the levels of aniline and p-nitroaniline in workplace air.Results Under the optimum analytical conditions,the detection limits of aniline and p-nitroaniline were 0.5μg/ml and 0.1μg/ml,respectively.The linearity in the linear ranges of aniline(0-50.0μg/ml)and p-nitroaniline(0-10.0μg/ml)was excellent,with correlation coefficients(r)both>0.999.The sample desorption efficiencies ranged from 96.40%-97.88%,the spiked recoveries ranged from 96.50%-99.17%,and the relative standard deviations(RSDs)of 2.37%-4.36%(n=6).There was no statistically significant difference between mass spectrometry and the national standard method for the detection of aniline and p-nitroaniline in air(F=0.007,0.065,t=0.084,0.256,P>0.05).Conclusion The method is easy to operate,with high target separation,good reproducibility and high sensitivity.It can be used as a daily detection method for aniline and p-nitroaniline in workplace air.

关 键 词：工作场所空气 苯胺 对硝基苯胺 超高效液相色谱-串联质谱 

分 类 号：R996[医药卫生—毒理学]