1. 中南大学化学化工学院
2. 湖南中烟工业有限责任公司
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万小红, 吴名剑, 蒋新宇, 等. 直接衍生/高效液相色谱法分析水基胶中羰基化合物[J]. 分析测试学报, 2011,30(12):1412-1418.
Analysis of Carbonyl Compounds in Water-based Adhesive by Direct Derivatization and High-performance Liquid Chromatography[J]. 2011,30(12):1412-1418.
建立了直接衍生/高效液相色谱分析水基胶中8种痕量羰基化合物(甲醛、乙醛、丙酮、丙烯醛、丙醛、丁烯醛、2-丁酮和丁醛)的方法。对影响分析效率的因素进行了考察,确定最佳衍生条件为:水基胶样品与2,4-二硝基苯肼衍生剂在40 ℃下反应20 min;最佳色谱分析条件为:采用DIONEX Acclaim Explosives E2反相柱,用水和乙腈进行二元梯度洗脱,流速1.2 mL/min,色谱柱温度35 ℃。8种羰基化合物的线性范围为0.001 1~55.32 mg/L,相关系数均大于0.999,方法的检出限为0.066 3~1.691 1 mg/kg,定量下限为0.221~5.637 mg/kg,相对标准偏差为4.3%~9.3%,回收率为62%~100%。该方法简单、灵敏、稳定、定量准确,能有效地分析水基胶中羰基化合物的含量。
A direct derivatization and high-performance liquid chromatographic method was developed for the trace analysis of 8 carbonyl compounds,e.g.formaldehyde,acetaldehyde,acetone,acrolein,propaldehyde,crotonaldehyde and 2-butanone and butaldehyde in water-based adhesive.The method adopted 2,4-dinitrophenylhydrazine(DNPH) to directly react with the adhesive sample solution,and the influence factors were investigated and optimized.The best derivatization condition was using the adhesive to react directly with DNPH at 40 ℃ for 20 min.The optimized chromatograpic conditions were as follows:DIONEX Acclaim Explosives E2 reversed-phase column as separation column,water and acetonitrile as mobile phase by double gradient elution.The flow rate was set at 1.2 mL/min,and the column temperature was set at 35 ℃.Under the optimal conditions,the linear ranges of 8 carbonyl compounds were all in 0.001 1-55.32 mg/L,with correlation coefficients higher than 0.999.The limits of detection for 8 carbonyl compounds were 0.066 3-1.691 1 mg/kg,and the limits of quantitation were 0.221-5.637 mg/kg.The relative standard deviations were between 4.3% and 9.3%,and the recoveries were 62%-100%.The established method was sensitive,simple and accurate,and was practical for the determination of 8 carbonyl compounds in wate-based adhesive.
直接衍生溶剂萃取高效液相色谱法羰基化合物水基胶
direct derivatizationsolvent extractionhigh-performance liquid chromatographycarbonyl compoundswater based adhesive
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