超声萃取-高效液相色谱法测定纺织品中二苯甲酮类防紫外线整理剂

摘要

This paper puts forward a novel method to extract and determine 8 diphenyl ketone anti-ultraviolet finishing agents in textiles by ultrasonic extraction coupled with high performance liquid chromatography ( HPLC ) . The samples were extracted and redissolved in methanol, separated with Eclipse XDB-C18 chromatographic column, determined by diode array detector and quantified by external standard method. This paper discussed the effects of selection of extraction solvent, the method detection limit and linear correlation, added recovery and precision as well as chromatographic conditions. The experimental result shows that good linearity (R2 >0. 99) is observed between 1. 0 and 10. 0μg/mL for all compounds. When added mass concentration is 5. 0, 10. 0 and 20. 0 mg/kg, the average recovery rate scope of cotton samples is 89 . 57% ~105 . 03%, and relative standard deviation ( RSD ) is 3 . 06% ~9 . 80%. The average recovery rate scope of polyester samples is 98 . 80% ~115 . 31%, and relative standard deviation (RSD) is 0. 94% ~5. 63%. The average recovery rate scope of nylon samples is 84. 48% ~118. 88%, and relative standard deviation (RSD) is 1. 06% ~12. 48%. The limit of detection (LOD) is 0. 06~0. 2 mg/kg and limit of quantitation (LOQ) is 0. 19~0. 67 mg/kg. The method is simple, sensitive and accurate, and is suitable for the qualitative and quantitative determination of 8 diphenyl ketone anti-ultraviolet finishing agents in textiles.%采用超声萃取结合高效液相色谱,建立了一种提取和测定纺织品中8种二苯甲酮类防紫外线整理剂的分析方法。样品经提取、定容,采用Eclipse XDB-C18色谱柱分离,二极管阵列检测器测定,外标法定量。讨论了提取溶剂的选择、方法检测限与线性相关性、添加回收率与精密度及色谱条件的影响。结果表明：在1.0~10.0μg/mL范围内线性关系良好(R2>0.99),在添加质量浓度为5.0、10.0、20.0 mg/kg 时,棉布样品平均回收率范围为89.57％~105.03％,相对标准偏差( RSD )为3.06％~9.80％；涤纶样品平均回收率范围为98.80％~115.31％,相对标准偏差(RSD)为0.94％~5.63％；尼龙样品平均回收率范围为84.48％~118.88％,相对标准偏差(RSD)为1.06％~12.48％,方法检出限(LOD)为0.06~0.2 mg/kg,方法定量限(LOQ)为0.19~0.67 mg/kg。该方法操作简便、灵敏、准确,适合纺织品中8种二苯甲酮类防紫外线整理剂的定性和定量分析。