高效液相色谱法测定空气中苯胺和N-甲基苯胺的研究

Study on HPLC Method for Determination of Aniline and N-methylaniline in Air

目的建立高效液相色谱法同时测定空气中苯胺、N-甲基苯胺的检测方法。方法应用高效液相色谱,C18通用色谱柱,以甲醇为流动相,流速0.7ml/min,紫外检测器在240nm波长下测定吸收值。结果苯胺线性范围0.00～1000μg/ml,回归方程:y=0.000936x+0.6769,相关系数r=0.9999,最低检出浓度1.0μg/ml,空气中最低检出浓度0.22μg/m3,在250、25、2.5μg/ml浓度下测得平均回收率分别为:99.2%、100.5%、104.4%,相对标准偏差RSD分别为0.23%、0.42%、3.25%;N-甲基苯胺线性范围0.00～1000μg/ml,回归方程:y=0.00124x+0.02,相关系数r=0.9999,最低检出浓度0.4μg/ml,空气中最低检出浓度0.09μg/m3,在250、25、2.5μg/ml浓度下测得平均回收率分别为:99.7%、101.6%、102.0%,相对标准偏差RSD分别为0.27%、0.23%、3.65%。结论分析时间短,相关性好,精密度高,准确度好,特异性强,该法线性范围宽。

Objective To develop a method for determination of aniline and N- methylaniline in air by HPLC. Methods The separation was carried out on a universal O18 column, methanol was used respectively as mobile phases in analyzing N- methylaniline. The flow rate was 0.7 ml/min, the detector was UV detector. The detective wavelength was set at 240 nm. Results The linearity of aniline was obtained over the range of 0.00-1000 μ/ml. The regression equation was y = 0. 000936x ＋ 0. 676, the correlation coefficient was 0. 9999. The limit of detection （LOD） was 1.0pg/ml, The limit of detection in air was 0.22μg/m^3 . The average recovery was 99.2 %, 100.5 %, and 104.4 % with RSD % （0.23 %, 0,42 %, and 3.25 %） when the sample concentration was 250pg/ml, 25μg/ml, and 2. 5μg/ml. The linearity of N - methylaniline was obtained over the range of 0.00- 1000μg/ml . The regression equation Was y = 0,00124x ＋ 0.02, the correlation coefficient was 0. 9999. The limit of detection （LOD） was 0.4μg/ml. The limit of detection in air was 0.09μg/m^3 . The average recovery was 99,7%, 101.6%, and 102.0% with RSD% （0.27%, 0.23%, and 3.05% ） when the sample concentration was 250μg/ml, 25μg/ml, and 2.5μg/ml. Conclusions The method is rapid, with good specificity for the determination of aniline and Nmethylaniline in air. The method is wide of linear range and is good of the correlation coefficient.