摘要
基于酸性介质中甲酸对高锰酸钾-苯二酚氧化发光反应的增敏作用建立了高效液相色谱-化学发光柱后检测苯二酚的新方法。优化了高锰酸钾-苯二酚氧化发光反应及高效液相色谱分离苯二酚的条件，用甲醇，0．1mmol／L β-环糊精水溶液（体积比为30：70）作为流动相可实现对水中3种苯二酚异构体的分离，且能与高锰酸钾-苯二酚氧化化学发光反应条件很好地偶合。对所测定的苯二酚异构体，方法的线性范围达两个数量级；以信噪比为3测得邻、间、对苯二酚的检出限（n=3）分别为：5．2，4．7，3．2μg／L，对质量浓度均为0．10mg／L的3种苯二酚混合溶液连续测定11次，邻、间、对苯二酚的相对标准偏差分别为2．8％，3．4％，6．5％。将该方法与固相萃取技术相结合，对河水中的痕量苯二酚进行了测定，加标回收率为92．1％～95．4％。
A sensitive, selective and simple post-column chemiluminescence （CL） detection method for simultaneously determining catechol, resorcinol, hydroquinone has been developed based on high performance liquid chromatography （HPLC） coupled with CL detection using reaction of dihydroxybenzenes with acidified potassium permanganate solution with the enhancing effect of formic acid. The optimal conditions for the CL detection and HPLC separation were achieved. Dihydroxybenzene isomers were baseline separated at column temperature of 25℃ using a mobile phase of methanol-0.1 mmol/L β-cyclodextrin aqueous solution （30/70, v/v） with an isocratic elUtion program and the mobile phase matched well the CL detection. For all compounds, the linear ranges of the CL detection were about two orders of magnitude. The detection limits were 3.2 μg/L for hydroquinone, 4.7 μg/L for resorcinol and 5.2 μg/L for catechol. Combining with solid phase extraction, the proposed method was successfully applied to the determination of dihydroxybenzenes in river water. The recoveries for the three dihydroxybenzenes were 92.196 - 95.4%.
出处
《色谱》
CAS
CSCD
北大核心
2006年第2期148-151,共4页
Chinese Journal of Chromatography
基金
国家自然科学基金项目(No.20437020)
中国科学院重要方向性研究项目(No.KZCX3-SW-432)
关键词
高效液相色谱
化学发光检测
高锰酸钾
固相萃取
苯二酚
high performance liquid chromatography （HPLC）
chemiluminescence （CL） detection
potassium permanganate
solid phase extraction （SPE）
dihydroxybenzenes
