提出了高效液相色谱法测定粉饼中8种苯胺类物质(苯胺、对硝基苯胺、3-硝基苯胺、对甲苯胺、间氯苯胺、2,4-二硝基苯铵、2-氯-4-硝基苯胺、4-氯-2-甲基苯胺)含量的方法。样品中8种苯胺类物质用甲醇超声提取,离心分离后,所得提取液过0.45 μm有机滤膜。以SinoChrom ODS-BP色谱柱(4.6 mm×200 mm,5 μm)为分离柱,不同比例配成的甲醇和水混合溶液为流动相梯度洗脱,用紫外-可见光检测器于波长254 nm处检测。方法的检出限(3S/N)在0.01~0.07 μg·g-1之间,相对标准偏差(n=10)均小于1%。以空白粉饼样品为基体,用标准加入法测定方法的回收率,结果在87.5%~118%之间。

Contents of 8 anilines (i.e., aniline, p-nitroaniline, 3-nitroaniline, p-toluidine, m-chloroaniline, 2,4-dinitroaniline, 2-chloro-4-nitroaniline and 4-chloro-2-methyl aniline) in pressed powder were determined by HPLC. The 8 anilines in the sample were extracted ultrasonically with methanol. After centrifugation, the extract was filtered on 0.45 μm organic filtering membrane. SinoChrom ODS-BP (4.6 mm×200 mm, 5 μm) chromatographic column was used as stationary phase, and solutions of methanol mixed with water in different ratios were used as mobile phase in the gradient elution. The eluate from the column was determined with UV-Vis detector at the wavelength of 254 nm. Detection limits (3S/N) of the method were found in the range of 0.01-0.07 μg·g-1, and RSD′s (n=10) found were less than 1%. Using blank sample of pressed powder as matrixes, values of recovery found by standard addition method were in the range of 87.5%-118%.