色谱 ›› 2011, Vol. 29 ›› Issue (02): 184-186.DOI: 10.3724/SP.J.1123.2011.00184

• 技术与应用 • 上一篇    下一篇

反相高效液相色谱法测定荧光增白剂CBS中N,N-二甲基甲酰胺的残留量

甘宏宇*, 张天玉   

  1. 山西青山化工有限公司, 山西 运城 044100
  • 收稿日期:2010-10-08 修回日期:2010-11-19 出版日期:2011-02-28 发布日期:2007-03-25
  • 通讯作者: 甘宏宇,博士.

Determination of residual N,N-dimethylformamide in fluorescent brightening agent CBS by reversed-phase high performance liquid chromatography

GAN Hongyu*, ZHANG Tianyu   

  1. Shanxi Qingshan Chemical Industry CO., LTD, Yuncheng 044100, China
  • Received:2010-10-08 Revised:2010-11-19 Online:2011-02-28 Published:2007-03-25

摘要: 建立了反相高效液相色谱外标法检测荧光增白剂CBS(即CF-351)中N,N-二甲基甲酰胺(DMF)残留量的方法。使用Accurasil C18(150 mm×4.6 mm,5 μm)反相液相色谱柱,以甲醇-水为流动相梯度洗脱,流速为1.0 mL/min,检测波长为205 nm,柱温为30 ℃,进样量为5 μL。在上述条件下,在DMF质量浓度为0.19~141 mg/L范围内,其峰面积与质量浓度的线性关系良好。在加标水平(用质量分数表示)为0.2344%和0.4678%时,回收率为98.4%~107.3%。本方法最低检出限(LOD)为0.019%(质量分数),峰面积的相对标准偏差(RSD)为1.73%。此方法可快速、准确地测定出荧光增白剂CBS中DMF的残留量。

关键词: N,N-二甲基甲酰胺, 残留量, 反相高效液相色谱, 荧光增白剂CBS

Abstract: A method for the determination of N,N-dimethylformamide (DMF) residue in fluorescent brightening agent CBS by reversed-phase high performance liquid chromatography (RP-HPLC) was established. An Ameritech Accurasil C18 column (150 mm×4.6 mm,5 μm) was used with methanol-water as the mobile phase with gradient elution. The flow rate of the mobile phase was 1.0 mL/min and the detection wavelength was 205 nm. The column temperature was 30 ℃ and the injection volume was 5 μL. There was a good linear relationship between the peak area and the concentration of DMF in the range of 0.19~141 mg/L. The recoveries of DMF were 98.4%~107.3% at the spiked levels of 0.2344% and0.4678%. The limit of detection was 0.019%. The relative standard deviation was 1.73%. This method can be used for the determination of DMF in fluorescent brightening agent CBS quickly and accurately.

Key words: fluorescent brightening agent CBS, N,N-dimethylformamide (DMF), residue, reversed-phase high performance liquid chromatography (RP-HPLC)

中图分类号: