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QuEChERS-超高效液相色谱法同时测定硝基酚类物质方法的研究
作者:
作者单位:

(1. 北京理工大学 爆炸科学与技术国家重点实验室, 北京 100081; 2. 潍坊市食品药品检验检测中心, 山东 潍坊 262500)

作者简介:

刘玉(1974-),博士研究生,主要从事硝基化合物含能材料研究。e-mail liuyufood@163.com 通信联系人: 张同来(1960-),男,教授,主要从事含能材料制备性能及应用研究。e-mail: ztlbit@bit.edu.cn

通讯作者:

张同来(1960-),男,教授,主要从事含能材料制备性能及应用研究。e-mail: ztlbit@bit.edu.cn

基金项目:

应用物理化学实验室科技基金(9140C3703051105,9140C370303120C37142)与爆炸科学与技术国家重点实验室基金(QNKT12-02)


Simultaneous Determination of 14 Nitrophenol Compounds by QuEChERS-Ultra Performance Liquid Chromatography
Author:
Affiliation:

(1. State Key Laboratory of Explosion Science and Technology, Beijing Institute of Technology, Beijing 100081, China; 2. Weifang Food and Drag Inspection and Testing Center Institute, Weifang 262511, China)

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    摘要:

    建立了超高效液相色谱法同时测定三硝基苯酚(苦味酸PA)、三硝基间苯二酚(斯蒂酚酸TNR)和三硝基均苯三酚(TNPG)等多硝基酚类含能材料在生产环境中土壤、地面沉积物中残留的14种硝基酚类物质的检测方法。样品经改进的QuEChERS(快速、简单、价廉、高效、耐用、安全)前处理方法一步完成提取, 经C18和石墨化炭黑(GCB)净化, 采用Accucore PFP色谱柱(2.1 mm×150 mm i.d., 2.6 μm)分离, 用梯度洗脱, 流动相为乙腈+0.02 mol·L-1乙酸铵盐缓冲溶液+0.1%甲酸, 流速0.3 mL·min-1, 注射量5 μL。在波长220 nm处检测14种硝基酚类物质。结果表明, 14种硝基酚类物质在0.2~50 mg ·L-1浓度范围内呈良好线性关系, 相关系数为0.9985~0.9995, 相对标准偏差为3.6%~5.9%, 平均回收率为81.3%~105.7%, 检出限(LOD)为0.04~0.06 mg·kg-1。14种硝基酚类物质在22 min内完成分离。所建方法有良好的重复性和精度, 可用于快速测定土壤中的酚类物质。

    Abstract:

    With an ultra performance liquid chromatography (UPLC), a method for simultaneous determination was established for fourteen nitrophenol residues including 2, 4, 6-trinitrophenol [picric acid (PA)], 2, 4, 6-trinitroresorcinol [styphnic acid (TNR)] and 2, 4, 6-trinitrophloglucinol (TNPG) remained in soil and ground sediment of production areas of energetic materials. The sample extraction was completed in one procedure via a modified QuEChERS(quick, easy, cheap, effective, rugged, safe) pretreatment method. The samples were purified by C18 and graphitized carbon black (GCB). Fourteen nitrophenol compounds were separated by an Accucore PFP (2.1 mm×150 mm i.d., 2.6 μm)column, and the radiant elution was employed with a mobile phase consisting of acetonitrile and 0.02 mol·L-1 ammonium acetate buffer solution, and 0.1% formic acid, a solvent flow rate of 0.3 mL·min-1 and an injection volume of 5 μL. Fourteen nitrophenol compounds were identified at 220 nm. Results show that fourteen nitrophenol samples were linear in the concentration range of 0.2-50 mg·L-1 with linear correlation coefficient ofof 0.9985-0.9995. The detection limits of the components were 0.04-0.06 mg·L-1, and the average recoveries are 81.3%-105.7% with relative standard deviations of 3.6%-5.9%. Fourteen nitrophenol compounds were separated within 22 min. The established method can be applied to the rapid determination of nitrophenols residues in soil with good repeatability and precision.

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刘玉,张同来,杨利,等. QuEChERS-超高效液相色谱法同时测定硝基酚类物质方法的研究[J].含能材料, 2015, 23(1):73-79. DOI:10.11943/j. issn.1006-9941.2015.01.015.
LIU Yu, ZHANG Tong-lai, YANG Li, et al. Simultaneous Determination of 14 Nitrophenol Compounds by QuEChERS-Ultra Performance Liquid Chromatography[J]. Chinese Journal of Energetic Materials, 2015, 23(1):73-79. DOI:10.11943/j. issn.1006-9941.2015.01.015.

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  • 收稿日期: 2014-03-06
  • 最后修改日期: 2014-03-28
  • 录用日期: 2014-04-28
  • 在线发布日期: 2015-01-20
  • 出版日期: 2015-01-20