色谱

色谱 ›› 2011, Vol. 29 ›› Issue (12): 1183-1187.DOI: 10.3724/SP.J.1123.2011.01183

• 研究论文 • 上一篇    下一篇

直接衍生离子液体富集高效液相色谱分析水基胶中脂肪族醛酮

万小红1, 吴名剑2, 蒋新宇1*, 戴云辉2, 李绍晔2, 龚淑果2   

  1. 1. 中南大学化学化工学院, 湖南 长沙 410083; 2. 湖南中烟工业有限责任公司, 湖南 长沙 410007
  • 收稿日期:2011-08-30 修回日期:2011-11-06 出版日期:2011-12-28 发布日期:2012-01-15
  • 通讯作者: 蒋新宇,副教授,主要从事手性药物分离和有机物质分析研究.
  • 基金资助:

    湖南省科技计划项目(No.2010WK3029)

Analysis of aliphatic aldehydes and ketones in water-based adhesive by direct derivatization-ionic liquid gathering coupled with high performance liquid chromatography

WAN Xiaohong1, WU Mingjian2, JIANG Xinyu1*, DAI Yunhui2, LI Shaoye2, GONG Shuguo2   

  1. 1. College of Chemistry and Chemical Engineering, Central South University, Changsha 410083, China; 2. Hunan Tobacco Industry Co., Ltd., Changsha 410007, China
  • Received:2011-08-30 Revised:2011-11-06 Online:2011-12-28 Published:2012-01-15

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摘要： 建立了以2,4-二硝基苯肼(DNPH)直接衍生,1-丁基-3-甲基咪唑六氟磷酸盐(［BMIM］PF6)萃取富集,高效液相色谱(HPLC)分析水基胶中痕量脂肪族醛酮的方法。分散的水基胶乳液用80 mg/L DNPH衍生化试剂(含0.44 mol/L磷酸)于40 ℃衍生18 min。取离心后的上层衍生液,加入0.5 mL ［BMIM］PF6于30 ℃萃取富集,离子液体相过滤后进行HPLC分析。采用Dionex Acclaim Explosives E2色谱柱(250 mm×4.6 mm, 5 μm),以水-乙腈为流动相在流速1.2 mL/min进行梯度洗脱,色谱柱温度为35 ℃,检测波长为365 nm。结果表明,8种脂肪族醛酮的检出限为0.022～0.221 mg/kg,定量限为0.073～0.738 mg/kg,相对标准偏差为3.5%～7.3%,回收率为84.0%～102.5%。与溶剂萃取法相比,该法具有检出限和定量限低、稳定性高、测定更准确的优势。

关键词: 高效液相色谱, 离子液体富集, 水基胶, 脂肪族醛酮, 直接衍生

Abstract: A novel method was developed for trace analysis of aliphatic aldehydes and ketones in water-based adhesive based on 2,4-dinitrophenylhydrazine (DNPH) direct derivatization-1-butyl-3-methylimidazolium hexafluorophosphate (［BMIM］PF6) preconcentration coupled with high performance liquid chromatography (HPLC). The dispersive water-based adhesive emulsion directly reacted with 80 mg/L DNPH solution containing 0.44 mol/L phosphoric acid at 40 ℃ for 18 min. After centrifuging, 0.5 mL ［BMIM］PF6 was added to extract the derivatives at 30 ℃. The ionic liquid (IL) phase was filtered and then analyzed by HPLC. The separation was achieved by using a Dionex Acclaim Explosive E2 column (250 mm×4.6 mm, 5 μm) under the gradient elution with acetonitrile and water as mobile phases at the flow rate of 1.2 mL/min. The column temperature was 35 ℃, and the detection wavelength was 365 nm. The results showed that the limits of detection (LODs) were 0.022~0.221 mg/kg, and the limits of quantification (LOQs) were 0.073~0.738 mg/kg. The relative standard deviations (RSDs) were in the range of 3.5%~7.3%, and the recoveries were 84.0%~102.5% for 8 aliphatic aldehydes and ketones. Compared with solvent extraction, the established method has the advantages of lower LOD and LOQ, and is more stable and precise. This method is practical for the determination of aliphatic aldehydes and ketones in water-based adhesives.

Key words: aliphatic aldehydes and ketones, high performance liquid chromatography (HPLC), ionic liquid gathering, water-based adhesive, direct derivatization