使用顶空单滴微萃取法测定纺织品中甲醛

Formaldehyde Test of Textile with Method of Headspace Solvent Microextraction

介绍基于顶空单滴微萃取结合高效液相色谱法测定纺织品中甲醛的新方法。对萃取剂(包括乙酰丙酮浓度、pH值、乙酸铵浓度和有机溶剂组成)、萃取衍生温度、NaCl浓度和萃取时间进行了优选。采用顶空单滴微萃取结合高效液相色谱法测定了纺织品中甲醛,并与紫外-可见光分光光度法和高效液相色谱法进行了对比。结果表明:在萃取剂pH=5、含1.5%(V/V)乙酰丙酮和3 mol/L乙酸铵的甘油-DMF溶液、萃取温度70℃、萃取时间2min、NaCl浓度25%(m/V)的条件下,顶空单滴微萃取结合高效液相色谱法的相对标准偏差(n=6)小于7%,检测限(以S/N=3)和定量限(以S/N=10)分别为1.2mg/kg和3.5mg/kg。认为:新方法可用于纺织品中甲醛含量的测定。

New method testing formaldehyde in textile based on headspace single drop microextraction combination with high efficiency liquid chromatography was introduced. Extraction agents extraction derived temperature,NaCl concentration and extraction time were optimized. Formaldehyde was tested by method of headspace single drop microextraction combination with high efficiency liquid chromatography. Results were compared with methods of ultraviolet-visible spectrophotometry and high efficiency liquid chromatography. The result shows that when extraction pH value is 5,glycerinum-DMF solution contains is 1.5 % acetylacetone and 3 mol/L ammonium acetate,extraction temperature is 70 ℃, extraction time is 2 min and NaC1 concentration is 25%, the relative standard deviation is less than 7 %. In addition,test limitation （considering S/N= 3） and limit of quantitation are 1.2 mg/kg and 3.5 mg/kg respectively. It is considered that the new method can be used for formaldehyde test in textiles.