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建立了气相色谱–质谱法测定玩具涂层中邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁苄酯(BBP)、邻苯二甲酸二(2?乙基己基)酯(DEHP)、邻苯二甲酸二正辛酯(DNOP)、邻苯二甲酸二异壬酯(DINP)、邻苯二甲酸二异癸酯(DIDP)等6种邻苯二甲酸酯类增塑剂的分析方法,确定了适宜的微波辅助萃取条件为:以二氯甲烷为萃取剂,萃取温度60°C,萃取时间25 min。在试验选定的条件下,以该方法测定玩具涂层中6种邻苯二甲酸酯类增塑剂,以峰面积对质量浓度线性回归,线性范围在0.5~50 mg/L,则相关系数大于0.999,最低检出限为0.5~1.0 mg/L,加标回收率在83.5%~105.6%之间,相对标准偏差小于5.8%。该方法操作简便快速,准确度和灵敏度高,适合于玩具涂层中6种邻苯二甲酸酯类增塑剂含量的同时测定。

A method for determining six kinds of phthalate plasticizers including dibutyl phthalate (DBP), benzyl butyl phthalate (BBP), bis(2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DNOP), di-iso-nonyl phthalate (DINP), and di-iso-decyl phthalate (DIDP) in coatings on toys by gas chromatography-mass spectrometry (GC-MS) was established. The conditions of microwave assisted extraction were optimized as follows:dichloromethane as extractant, extraction temperature 60 °C, and extraction time 25 min. Under the selected experimental conditions, six phthalate plasticizers in coatings on toys were determined by the method, and the linear regression between peak area and mass concentration of individual plasticizer was made. The linear range is 0.5-50 mg/L, correlation coefficient higher than 0.999, detection limit 0.5-1.0 mg/L, recovery of standard addition 83.5%-105.6%, and relative standard deviation less than 5.8%. The method is easy and rapid to operate with good accuracy and sensitivity, suitable for simultaneous determination of the concentrations of six phthalate plasticizers in coatings on toys.

参考文献

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