响应面优化-气相色谱串联质谱法测定塑胶跑道面层中4种新型增塑剂

GC-MS/MS Determination of Four Emerging Plasticizers in Plastic Track Surface with Response Surface Methodology

基于气相色谱-串联质谱法(GC-MS/MS)建立了测定塑胶跑道面层中4种新型增塑剂的检测方法。剪碎后的跑道面层样品经20 mL乙酸乙酯于62℃、180 W超声提取41 min,过0.22μm聚四氟乙烯(PTFE)滤膜,目标物经TG-5SilMS色谱柱分离,在电子轰击源(EI)下进行选择反应监测(SRM),外标法定量。基于Box-bennken设计了响应曲面,得到超声提取法中超声温度、超声时间、超声功率的最佳值。结果表明:在0.05~2.00 mg/L线性范围内,4种新型增塑剂的相关系数(r^(2))均大于0.999,检出限(LOD)为0.4~0.8 mg/kg,平均加标回收率为95.5%~114.5%,相对标准偏差(RSD)为2.3%~5.8%(n=6)。运用该方法对30批次塑胶跑道面层样品进行检测。结果23批次样品均检出新型增塑剂,其中对苯二甲酸二辛酯(DOTP)的检出率高达66.7%,最高检出浓度为6.3×10^(3)mg/kg。该方法简便、准确,适用于检测塑胶跑道面层中4种新型增塑剂。

A method for the determination of four emerging plasticizers in plastic track surface was developed by gas chromatography-tandem mass spectrometry(GC-MS/MS).The shredded plastic track surface were extracted by ultrasonic extraction with 20 mL ethyl acetate at 62℃and 180 W for 41 min,and filtered through 0.22μm polytetrafluoroethylene(PTFE)membrane.The target compounds were separated by TG-5SilMS column,and then determined by selective reaction monitoring(SRM)mode under electron bombardment source(EI),and quantified by external standard method.The response surface methodology(RSM)based on Box-Behnken design was used to determine the optimal values of ultrasonic temperature,ultrasonic time,and ultrasonic power in the ultrasonic extraction method.The results showed that the correlation coefficients(r^(2))of four emerging plasticizers were all over than 0.999 in the linear range of 0.05~2.00 mg/L,the limits of quantification(LOD)were 0.4~0.8 mg/kg,the average recoveries ranged from 95.5%to 114.5%,with relative standard deviations(RSD)of 2.3%~5.8%(n=6).This method was used to detect 30 batches of plastic track surface.As a result,the emerging plasticizers were detected in 23 batches of plastic track surface in varying degrees.The highest detection rate of DOTP was 66.7%,and the highest detection concentration of DOTP was 6.3×10^(3) mg/kg.The method was simple,accurate,and suitable for the determination of four emerging plasticizers in plastic track surface.