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OA北大核心CSTPCD
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0.22 μm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(r2)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6.3×103 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 0.22 μm 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(r2)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 6.3×103 mg/kg.The method was simple,accurate,and suitable for the determination of four emerging plasticizers in plastic track surface.
杨倩;冉露;唐怡佳;余秋玲;张念;陆嘉莉
重庆市计量质量检测研究院,重庆 401123重庆化工职业学院,重庆 401228
化学
对苯二甲酸二辛酯气相色谱-串联质谱法塑胶跑道面层响应曲面法
Dioctyl terephthalateGC-MS/MSPlastic track surfaceResponse surface methodology
《塑料科技》 2024 (006)
115-121 / 7
重庆市科技局科研院所绩效激励引导专项(cstc2022jxjl50001);重庆市市场监督管理局科研计划项目(CQSJKJ2021041)
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