色谱

色谱 ›› 2014, Vol. 32 ›› Issue (3): 230-234.DOI: 10.3724/SP.J.1123.2013.11028

• 研究论文 • 上一篇    下一篇

柱前衍生高效液相色谱法同时测定水性涂料中6种醛类化合物

陈潜1, 周宇艳2, 程欲晓2, 林苗1   

  1. 1. 东华大学化学化工与生物工程学院, 生态纺织教育部重点实验室, 上海 201620;
    2. 上海出入境检验检疫局工业品与原材料检测技术中心, 上海 200135
  • 收稿日期:2013-11-14 修回日期:2013-12-11 出版日期:2014-03-08 发布日期:2014-03-04
  • 通讯作者: 林苗
  • 基金资助:

    国家质检总局“双打”质检公益专项基金项目（2012104020）.

Simultaneous determination of six aldehydes in water-based coatings by high performance liquid chromatography with pre-column derivatization

CHEN Qian1, ZHOU Yuyan2, CHENG Yuxiao2, LIN Miao1   

  1. 1. College of Chemistry, Chemical Engineering and Biotechnology, Donghua University, Key Laboratory of Science & Technology of Eco-Textile (Donghua University), Ministry of Education, Shanghai 201620, China;
    2. Technical Center for Industrial Products and Raw Materials Inspection, Shanghai Entry-Exit Inspection and Quarantine Bureau, Shanghai 200135, China
  • Received:2013-11-14 Revised:2013-12-11 Online:2014-03-08 Published:2014-03-04

PDF

296

被引次数

7

摘要：

建立了柱前衍生高效液相色谱同时测定水性涂料中甲醛、乙醛、丙醛、苯甲醛、正戊醛和对甲基苯甲醛等6种醛类化合物的方法。样品经水超声提取后，与2，4-二硝基苯肼乙腈溶液在酸性条件下衍生，再经0.45 μm针式过滤器过滤后进样分析。系统考察了酸度调节剂、pH值、反应温度、时间等因素对衍生反应的影响，优化的反应条件为：以稀释后的盐酸溶液作为酸度调节剂，缓冲溶液pH=3，反应温度为60 ℃，反应时间为30 min。在此条件下，于0.08~2.0 mg/L浓度范围内，6种醛类化合物呈良好的线性关系；检出限为0.05~2.50 mg/kg；在2.0、4.0、6.0 mg/kg 3个水平下的加标回收率为87.0%~112.8%；RSD为1.12%~9.54%。结果表明，本方法具有较宽的线性范围，良好的精密度和准确度，适用于水性涂料中6种醛类化合物的同时测定。

关键词: 2,4-二硝基苯肼, 高效液相色谱法, 醛类化合物, 水性涂料, 柱前衍生

Abstract:

A high performance liquid chromatography method with pre-column derivatization was developed for the simultaneous determination of formaldehyde, acetaldehyde, propionaldehyde, benzaldehyde, n-valeraldehyde and p-tolualdehyde in water-based coatings. After ultrasonic extraction with water, the samples were derivatized with 2,4-dinitrophenylhydrazine (2,4-DNPH) in acetonitrile under acidic condition, then filtrated by 0.45 μm organic syringe filters for the determination. Systematic investigation was carried out on the dependence of the derivatization conditions such as the acidity regulator, pH value, reaction temperature, reaction time and other factors. The optimized conditions were as follows: the dilute hydrochloric acid solution as acidity regulator, the pH of the buffer solution of 3, the reaction temperature of 60 ℃, and the reaction time of 30 min. Under the conditions, a linear relation was achieved in the range of 0.08-2.0 mg/L for the peak area to concentration of the six aldehydes. The detection limits were 0.05-2.50 mg/kg. The recoveries of standard addition at the spiked levels of 2.0, 4.0, 6.0 mg/kg were 87.0%-112.8% with the relative standard deviations (RSDs, n=6) of 1.12%-9.54%. The results showed that this method has a wide linear range, good precision and accuracy, and it is suitable for the simultaneous determination of the six aldehydes in water-based coatings.

Key words: 2,4-dinitrophenylhydrazine, aldehydes, high performance liquid chromatography (HPLC), pre-column derivatization, water-based coatings

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