摘要
建立了采用乙酰丙酮-乙酸铵-乙酸试剂衍生后再用HPLC法将多种醛类与衍生试剂反应后的产物用HPLC分离,快速准确检测皮革中甲醛含量的分析方法。考察了乙酰丙酮、乙酸铵试剂,衍生反应条件及衍生产物的稳定性。用乙酰丙酮、乙酸铵试剂柱前衍生,产物经XDB-C18柱(4.6mm×250mm,5μm)柱分离,采用可变波长扫描紫外检测器检测,检测波长412nm;流动相为(乙腈)颐(水)=30颐70(/V),流速为0.8mL/min。方法在0.05~80.0mg/L范围内线性关系良好,相关系数为0.9998,加标回收率为90%~98%,RSD小于5%,检测限为0.01mg/L(S/N=3),可完全满足皮革中甲醛测试的要求。
Formaldehyde content in leather was analyzed by High-performance liquid chromatography through derivatization with acetylacetone and ammonium acetate reagent. Factors such as amount of derivatization reagent, derivatization conditions and stability of derivative were studied. The results indicated that derivative could be well separated by C18 column (4.6 mmx 250 mm, 5 p,m), with acetonitrile-water (30:70 (V/V)) as mobile phase at flow rate of 0.8 mL/min. Target derivative then could be well detected by UV detector at wavelength 412 nm. Response peak and amount of formaldehyde has good linear relationship with the coefficient of 0.9998 when the amount of formaldehyde is between 0.05 mg/L and 80.0 mg/L. The RSD value is 〈5%. The detection limit is 0.01 mg/L (S/N=3), which can fully meet the detection requirement of formaldehyde in leather.
出处
《西部皮革》
2013年第2期47-50,共4页
West Leather
关键词
试剂柱前衍生
皮革
甲醛
高效液相色谱法
pre-column derivatization
leather
formaldehyde
high performance liquid chromatography