乙酰丙酮液质联用法测定纺织品中的甲醛

Detection of formaldehyde in textiles using acetylacetone-HPLC-MS/MS method

为了高效、灵敏地检测纺织品中甲醛的含量,建立了一种乙酰丙酮液质联用法,并探究提取条件、色谱条件和质谱条件对该方法测试结果的影响,对测试条件进行了优化,最终得出最佳测试条件。样品提取液经超声萃取后进行衍生化,使用InfinityLab Poroshell 120 EC-C182.7μm×3.0 mm×150 mm色谱柱、乙腈:水为流动相对经乙酰丙酮衍生化的提取液进行梯度洗脱,而后经质谱进行测定,以特征离子定性,外标法进行定量。结果表明,甲醛在0.001~5.000μg/mL范围内具有良好的线性,相关系数R=0.9996,检出限为0.1768μg/kg,相对标准偏差<3%,加标回收率的范围为93.1%~97.7%。该方法准确性好,灵敏度高,为甲醛测定提供了新的方法和研究思路。

An acetylacetone-HPLC-MS/MS method was developed for the efficient and sensitive detection of formaldehyde in textiles,and the influence of extraction conditions,chromatographic conditions and mass spectrometry conditions on the test results of this method was explored,the test conditions were optimized,and the optimal test conditions were obtained.The sample extraction solution after ultrasonic extraction was derivatized.The extraction solution derived from acetylacetone extract was gradiented elution using the column:InfinityLab Poroshell 120 EC-C182.7μm×3.0 mm×150 mm and mobile phase of acetonitrile/water.Subsequently,the qualitative and quantitative analysis of the product was accomplished via the HPLC-MS/MS.The results show that a good linear relationship of formaldehyde ranging from 0.001μg/mL to 5.000μg/mL was established with R=0.9996 and the limit of detection(LOD)was 0.1768μg/kg.In addition,the relative standard deviation(RSD)was less than 3%and the range of recoveries was between 92.57%-97.47%.The developed method with high accuracy and sensitivity provides a new method and idea for the detection of formaldehyde.