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建立了煤沥青中苯并[a]蒽、苯并[a]芘等16种多环芳烃(PAHs)的高效液相色谱分离检测方法。以甲苯为溶剂对煤沥青进行萃取,萃取液处理后经柱层析分离,层析洗脱液分组回收,然后进行液相色谱分析。采用ZORBAX Eclipse PAH柱分离,以乙腈-水为流动相进行梯度洗脱,紫外检测器进行测定。结果表明,16种PAHs的线性范围为0.5~20 mg/L,相关系数(r)均大于0.999,检出限为0.0031~0.035μg/L,方法的回收率为97.2%~108.3%,相对标准偏差(RSD)为0.18%~3.5%。方法用于两种不同煤沥青中16种PAHs含量的测定,两种煤沥青中16种PAHs的含量分别为107.86 g/kg和103.71 g/kg,其中苯并[a]芘的含量分别为11.86 g/kg和13.82 g/kg。
A high performance liquid chromatographic separation and detection method for 16 kinds of polycyclic aromatic hydrocarbons (PAHs) such as benzo [a] anthracene and benzo [a] pyrene in coal tar pitch was established. Toluene was used as solvent to extract coal tar pitch. The extract was treated with column chromatography and separated by column chromatography. Then the liquid chromatographic analysis was carried out. The separation was carried out on a ZORBAX Eclipse PAH column, gradient elution with acetonitrile-water as mobile phase, and UV detector. The results showed that the linear range of 16 PAHs was 0.5 ~ 20 mg / L, the correlation coefficient (r) was greater than 0.999, the detection limit was 0.0031 ~ 0.035 μg / L, the recovery rate was 97.2% -108.3% Deviation (RSD) is 0.18% ~ 3.5%. The method was applied to the determination of 16 PAHs in two different coal tar pitches. The contents of 16 PAHs in the two kinds of coal tar pitch were 107.86 g / kg and 103.71 g / kg, respectively, of which the content of benzo [a] pyrene was 11.86 g / kg and 13.82 g / kg.