加速溶剂萃取-固相萃取-气相色谱/质谱法同时测定纺织固废物中两类塑化剂

Simultaneous Determination of Two Types of Plasticizers in Textile Solid Waste by Accelerated Solvent Extraction-Solid Phase Extraction-Gas Chromatography/Mass Spectrometry

建立了加速溶剂萃取-固相萃取-气相色谱/质谱(ASE-SPE-GC/MS)联用技术同时测定纺织原料类固废物中邻苯二甲酸酯和己二酸酯。探讨了萃取过程中不同萃取溶剂、萃取温度、静态萃取时间,以及固相萃取净化中洗脱液强度和体积对邻苯二甲酸酯和己二酸酯萃取率的影响。优化条件为:以正己烷为萃取剂,萃取温度100℃,静态萃取时间5 min,洗脱液为正己烷∶二氯甲烷=4∶1(V/V),洗脱体积10 mL。在筛选的实验条件下,14种目标物的回收率为89%~108%,相对标准偏差(RSD)为0.16%~2.7%,检出限为0.06~0.48 mg/kg。

In this work,we established an effective detection method for simultaneously determination of phthalates and adipates in solid wastes such as textile raw materials by combing the accelerated solvent extraction(ASE) and solid phase extraction(SPE) with GC/MS.The effects of different extraction solvents,extraction temperature,static extraction time,and the strength and volume of the eluent on the extraction of phthalate and adipate were discussed.Experimental results showed that the extraction efficiency was the best with n-hexane as the extractant,extraction temperature of 100 ℃,static extraction time of 5 min,eluent of n-hexane∶dichloromethane(4∶1,V/V),and elution volume of 10 mL.Under the optimized experimental conditions,85% to 108% recoveries of the 14 target compounds,0.16% to 2.7% of the relative standard deviations,and the limits of dectection were 0.06 to 0.48 mg/kg were obtained.