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作 者:汤莹 TANG Ying(SEP Analytical Services(Shanghai)Co.,Ltd.,Shanghai200109,China)
机构地区:[1]实朴检测技术(上海)股份有限公司,上海201109
出 处:《化学分析计量》2022年第8期44-48,共5页Chemical Analysis And Meterage
摘 要:建立气相色谱-质谱法同时测定塑胶跑道中3,3’-二氯一4,4’-二氨基二苯甲烷和6种邻苯二甲酸酯类增塑剂含量。样品以乙酸乙酯超声提取后,经DB-5MS色谱柱(30 m×0.25 mm,0.25μm)分离,采用气相色谱-质谱法进行定性和定量分析。邻苯二甲酸二丁酯、邻苯二甲酸丁二卞酯、3,3’-二氯一4,4’-二氨基二苯甲烷、邻苯二甲酸二乙基己酯、邻苯二甲酸二正辛酯的质量浓度在0.25~10 mg/L范围内线性良好,邻苯二甲酸二异壬酯、邻苯二甲酸二异癸酯在0.625~25 mg/L范围内线性良好,相关系数均大于0.995;3,3’-二氯一4,4’-二氨基二苯甲烷的检出限为0.38 mg/kg,样品加标回收率为83.3%~116.8%,测定结果的相对标准偏差为1.9%~3.5%(n=6);6种邻苯二甲酸酯类增塑剂检出限为0.6~3.6 mg/kg,样品加标回收率为84.0%~111.6%,测定结果的相对标准偏差为3.5%~9.1%(n=6)。该方法简便快速,准确度高,检出限低,满足定量分析要求。A gas chromatography-mass spectrometry(GC-MS)was developed for the simultaneous determination of 3,3’-Dichloro-4,4’-diaminodiphenylmethane(MOCA)and six phthalate plasticizers in plastic tracks.After ultrasonic extraction with ethyl acetate,the samples were separated by DB-5MS column(30 m×0.25 mm,0.25μm),and qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry.The mass concentrations of MOCA and 4 phthalates including dibutyl phthalate(DBP),benzyl butyl phthalate(BBP),bis(2-ethylhexyl)phthalate(DEHP),di-n-octyl phthalate(DNOP)had a good linear relationship with the chromatographic peak area in the range of 0.25-10 mg/L,di-iso-nonyl phthalate(DINP)and di-iso-decyl phthalate(DIDP)had a good linear relationship with the chromatographic peak area in the range of 0.625-25 mg/L,the correlation coefficients were all more than 0.995.The detection limits of MOCA were 0.38 mg/kg,the recoveries of the standard addition were 83.3%-116.8%,and the relative standard deviation of determination results was 1.9%-3.5%(n=6).The detection limits of six phthalate plasticizers were 0.6-3.6 mg/kg,the recoveries of the standard addition were 84.0%-111.6%,and the relative standard deviation of determination results was 3.5%-9.1%(n=6).The method is simple,rapid,high accuracy and low detection limit,which can meet the requirements of quantitative analysis.
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