直接衍生/高效液相色谱法分析水基胶中羰基化合物

Analysis of Carbonyl Compounds in Water-based Adhesive by Direct Derivatization and High-performance Liquid Chromatography

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 ExplosivesE2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 waterbased adhesive.