高效液相色谱法测定工作场所空气中二苯胺

Detecting diphenylamine in workplace air by high performance liquid chromatography

目的建立工作场所空气中二苯胺的高效液相色谱(HPLC)测定方法。方法采用硅胶管采集工作场所空气中二苯胺,经甲醇解吸,采用C18色谱柱分离,以去离子水∶甲醇(20∶80,V/V)为流动相洗脱,在二极管阵列检测器检测波长为285 nm的紫外光谱下,经HPLC仪测定。结果二苯胺在质量浓度为1. 85~184. 50 mg/L时线性关系良好,相关系数为0. 999 6;检出限为0. 07 mg/L,最低检出浓度为0. 02 mg/m3(以采集12. 0 L空气计);平均解吸效率为97. 70%~99. 61%;批内相对标准偏差(RSD)为0. 42%~3. 60%,批间RSD为1. 63%~2. 36%。样品在常温下可保存14 d以上。结论本方法操作简单、灵敏度高、线性范围宽,适用于工作场所空气中二苯胺的测定。

Objective To establish a method for detecting diphenylamine in workplace air by high performance liquid chromatography（ HPLC） method. Methods The diphenylamine in workplace air was collected by silica gel solid sorbent tube,desorbed with methanol,separated by C18 column,eluted with deionized water ∶ methanol（ 20 ∶ 80,V/V） as mobile phase,and its wavelength detected in diode array detector. It was determined by HPLC on the ultraviolet spectrum of285 nm. Results The good linearity range of diphenylamine was 1. 85-184. 50 mg/L. The correlation coefficient was0. 999 6. The detection limit was 0. 07 mg/L. The minimum detectable concentration was 0. 02 mg/m^3（ air sample volume of 12 L）. The average desorption efficiencies was 97. 70%-99. 61%. The within-run relative standard deviation（ RSD）and the between-run RSD were 0. 42%-3. 60% and 1. 63%-2. 36%,respectively. The samples could be stored at room temperature for at least 14 days. Conclusion This method is simple in operation,with high sensitivity and wide linear range. It is suitable for detecting diphenylamine in workplace air.