色谱

色谱 ›› 2012, Vol. 30 ›› Issue (12): 1282-1286.DOI: 10.3724/SP.J.1123.2012.07037

• 技术与应用 • 上一篇    下一篇

并联式双三元高效液相色谱系统快速检测土壤中6种蒽醌类化合物

马浩, 贺伟, 杨柳, 尹雪梅, 王文佳, 施超欧*   

  1. 华东理工大学分析测试中心, 上海 200237
  • 收稿日期:2012-07-19 修回日期:2012-09-26 出版日期:2012-12-28 发布日期:2012-12-19
  • 通讯作者: 施超欧,高级工程师,研究方向为离子色谱、液相色谱的开发与应用. E-mail: HPLC@ecust.edu.cn.

Determination of six anthraquinone compounds in soil by parallel type dual gradient high performance liquid chromatography

MA Hao, HE Wei, YANG Liu, YIN Xuemei, WANG Wenjia, SHI Chaoou*   

  1. Analysis and Research Center, East China University of Science and Technology, Shanghai 200237, China
  • Received:2012-07-19 Revised:2012-09-26 Online:2012-12-28 Published:2012-12-19

PDF

340

被引次数

17

摘要： 建立了用于住宅建设污染土壤中1,8-二硝基蒽醌、1,5-二硝基蒽醌、1-氨基蒽醌、蒽醌、萘、1,4,5,8-四氯蒽醌等6种蒽醌类化合物含量的高效液相色谱分析方法。利用Ultimate双三元液相色谱仪的特点,设计了一套并联式双系统,采用2根相同的色谱柱(Dikma Diamonsil C18)交叉分析,节省了41.46%的分析时间。以50 mL N,N-二甲基甲酰胺-1,4-二氧六环-甲醇(5:20:25, v/v/v)为萃取剂,采用超声波辅助方法提取样品中的6种目标物。6种目标物的平均加标回收率为82.7%～101%,相对标准偏差为1.8%～3.2%,检出限(以信噪比为3计)为0.007～0.054 mg/kg,可满足北京地方标准DB11/T 811-2011的限量要求。该方法简便、准确,并能节省检测时间,有良好的重现性,可用于土壤中蒽醌类化合物的检测。

关键词: 并联式双梯度, 蒽醌类化合物, 高效液相色谱, 土壤

Abstract: A high performance liquid chromatography (HPLC) was established for the determination of six anthraquinone compounds, 1,8-dinitroanthraquinone, 1,5-dinitroanthraquinone, 1-aminoanthraquinone, anthraquinone, naphthalene, 1,4,5,8-tetrachlorodibenzo anthraquinone, in polluted soil of residential construction. In this method, by using an Ultimate dual gradient liquid chromatograph (DGLC), designing a set of parallel dual system and accepting two same Dikma Diamonsil C18 columns (150 mm×4.6 mm, 5 μm) to cross-analysis, 41.46% of the analysis time can be saved. By using assisted ultrasonication to the extraction of the six substances in the samples with 50 mL N,N-dimethyl-formamide/1,4-dioxane/methanol (5/20/25, v/v/v), the average recoveries of the six analytes spiked in nine blank soil samples were 82.7%~101% with the relative standard deviations (RSDs) of 1.8%~3.2% and the limits of detection were 0.007~0.054 mg/kg, which can reach the limited requirement of the local standard in Beijing of DB11/T 811-2011. With the advantages of accessibility, high sensitivity and good reproducibility, this method can be used in the determination of anthraquinone compounds in soil.

Key words: anthraquinone compounds, parallel type dual gradient, soil, high performance liquid chromatography (HPLC)