摘要
建立了高效液相色谱-柱后衍生法测定日化用品中游离甲醛的方法。对测定条件如流动相、色谱柱、检测波长、衍生反应器体积、衍生剂流速等进行优化。该方法加标回收率为99.4%~104.9%,相对标准偏差小于2.3%(n=5)。与传统方法对比,该方法能够有效消除甲醛缓释剂、萃取剂不纯和颜色干扰的影响;可有效防止甲醛检测假阳性结果的产生,能更准确地体现样品中游离甲醛的质量分数,可用于表面活性剂及其制品中游离甲醛的检测。
A method was established to determine free formaldehyde in detergent by post-column derivatization high performance liquid chromatography. Experiment conditions such as mobile phase, chromatographic column, detection wavelength, derived reactor volume, derivative flow rate were optimized. The recovery of the method ranged from 99.4% to 104.9%, the relative standard derivation(RSD) of detection results was less than 2.3%(n=5). By comparison with the classic method, this method could effectively eliminate the influence of formaldehyde slow release agent, extractant impurity and color interference. This method could effectively prevent the false positive results of formaldehyde detection, accurately reflected the mass fraction of free formaldehyde in samples, and could be used for the detection of free formaldehyde in surfactants and their products.
引文
[1]中华人民共和国卫生部.化妆品安全技术规范(2015版)[S].
[2]于世林.高效液相色谱方法及应用[M].北京:化学工业出版社,2005:83.
[3]王萍,柳玉红.我国化妆品用防腐剂及分析方法的研究进展[J].环境与健康杂志,2007,24(7):557-559.
[4]KIBA N,SUN L,YOKOSE S,et al.Determination of nano-molar levels of formaldehyde in drinking water using flow-injection system with immobilized formaldehyde dehydrogenase after off-line solid-phase extraction[J].Analytica Chimica Acta,1999,378(1-3):169-175.
[5]国家环保局《水和废水监测分析方法》编委会.水和废水监测分析方法[M].北京:中国环境科学出版社,1998:413-317.
[6]杭世平.空气中有害物质的测定方法[M].第二版.北京:人民卫生出版社,1986:300.
[7]环境保护部.环境监测分析方法标准制修订技术导则(HJ268-2010)[S].