高效液相色谱法测定水中痕量酚类化合物研究

Determination of Trace Phenols in Water by HPLC

[目的]建立高效液相色谱法分析水中7种酚类化合物的检测方法。[方法]水中7种酚类化合物首先通过MN Chroma bond easy固相萃取小柱预分离和富集,以甲醇作为洗脱液,然后经氮吹浓缩后进入高效液相色谱仪进行分离及测定。[结果]色谱分析条件：色谱柱为ZORBAXEclipse XDB C8（4.6 mm×150.0 mm,5μm）;流动相为甲醇（B）和1%醋酸溶液（C）;梯度洗脱程序为0~6 min,B从35%上升至45%,6~12 min,升至60%,12~18 min,升至80%,18~22 min,升至90%;流速为0.70 ml/min;进样量为10μl,柱温为35℃。各目标组分在0.5~31.5 mg/L范围内其峰面积与质量浓度成良好的线性关系,r≥0.999 8;7种酚类化合物的RSD在1.78%~4.02%（n=6）,除苯酚外,其余6种酚类化合物的加标回收率在89.5%~106.0%。[结论]该方法具有操作简单、灵敏度高、方法重现性好等优点,可用于水中痕量酚类化合物的检测。

[Objective] The detection method of seven kinds of phenolic compounds in water by HPLC was built.[Method] Seven kinds of phenolic compounds from water samples were separated and enriched by using SPE column（MN Chroma bond easy） with methol as elution,then concentrated by N2,and finally isolated and determined by HPLC.[Result] The chormatograph conditions were as follows：a Zorbax xdbC8 column（4.6 mm × 150.0 mm,5 μm） was adopted,and the mobile phase consisted of methol（B） and 1% acetic acid solution（C） at a flow rate of 0.7 ml/min.The gradient program was：B from 35% to 45% in 0-6 min,to 60% in 6-12 min,to 80% in 12-18 min,and then to 90% in 18-22 min.10 μl sample was injected and the oven temperature was 35 ℃.The linear range of 7 kinds of phenolic compounds was 0.5~31.5 mg/L（r≥0.999 8）.The RSD of 7 kinds of phenolic compounds were 1.78%~4.02%（n=6）;The average recovery for 6 kinds of phenolic compounds except phenol were 89.5%-106.0%.[Conclusion] The method has some advantages of simple operation,high sensitivity and good method repeatability,so it could be used for the determination of trace phenols in water.