摘要
目的建立工作场所空气中3,4-二硝基呋咱基氧化呋咱（DNTF）的高效液相色谱测定方法。方法采用ODSC18柱（4.6 mm×200 mm×5μm）仪器为美国HP1100型高效液相色谱仪,紫外检测器,波长为216 nm,流动相为甲醇∶水=60∶40,流速为1.0 ml/min。结果检测限为0.012μg/ml（进样10μl洗脱液）,最低检出浓度为0.000 2 mg/m3（以采集150 L空气样品计）。回归方程为y=22.74x-56.05,相关系数r=0.999 5,高、中、低3个浓度的样品,6次重复测定,RSD为0.71%~1.28%,洗脱效率为94.08%~104.75%,方法的回收率为96.80%~100.11%;样品在室温至少可保存7 d;在该条件下与DNTF可能共存的三硝基甲苯、黑索今、奥克托今等不干扰测定。结论该方法各项指标均达到《工作场所空气中毒物检测方法的研制规范》的要求,适用于工作场所空气中3,4-二硝基呋咱基氧化呋咱的样品纯度的检测。
Objective To establish a method for the determination of 3,4-dinitrofurazanfuroxan（DNTF） in workplace air by high performance liquid chromatography（HPLC）.Methods HPLC was carried out in the ODS C18 pillars（4.6 mm×200 mm×5 μm）with methanol-water（60∶40）as a mobile phase of current velocity 1.0 ml/min,the detective wavelength was 216 nm.Results The limit of the method was 0.012 μg/ml（resent 10 μl eluent）.The lowest concentration limit was 0.000 2 mg/m3（150 L air for test sample）.Regression equation was y=22.74x-56.05（r= 0.999 5）.The relative standard deviation was 0.71%-1.28%,the elution efficiency was 94.08%-104.75%,the recovery rate was 96.80%-100.11%.The samples could be stored for at least 7 days at room temperature,and DNTF wasn＇t interfered to determine with TNT,DNT,RDX,HMX.Conclusion HPLC methods has the characteristics of simple sample handling,rapid determination,high sensitivity and good reproducibility,it could be used for determining DNTF in workplace air.
出处
《中国卫生工程学》
CAS
2010年第5期366-368,共3页
Chinese Journal of Public Health Engineering
基金
2001年兵器工业集团总公司立项科研课题(42001100203)
