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作 者:陈惠[1] 贾蕊[1] 贾丽[2] 朱若华[1] 汪瑗[1]
机构地区:[1]首都师范大学化学系,北京100037 [2]北京市理化分析测试中心,北京100089
出 处:《分析科学学报》2007年第1期21-24,共4页Journal of Analytical Science
摘 要:采用胶束电动毛细管色谱法对5种邻苯二甲酸酯类化合物(邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP))和邻苯二甲酸二正辛酯(DOP))进行了分离研究,考察了溶液的pH值、胶束浓度和有机改性剂等对分离的影响。结果表明:以5mmol/L硼砂-25mmol/L十二烷基硫酸钠(SDS)-15%(体积分数)甲醇溶液为电泳缓冲液(pH9.2),采用压力进样方式,25kV恒压下进行分离,在波长200nm处检测,各组分在17min内可达到基线分离。DMP、DEP、DBP、DEHP和DOP的检出限分别为0.13mg/L、0.14mg/L、0.38mg/L、0.13mg/L和0.10mg/L。本法应用于塑料食品袋中邻苯二甲酸酯类化合物的测定,回收率范围为81.80%~118.87%,峰面积的相对标准偏差(RSD)小于4.30%(n=10),测定结果满意。Five phthalate esters, namely dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate(DBP) ,di(2-ethylhexyl) phthalate (DEHP) and di-n-octyl phthalate (DOP) were separated by micellar electrokinetic capillary chromatography. The effects of experimental parameters includeing pH, the contents of surfactant and organic modifier on the separation were investigated. The optimum electrophoretic conditions were as follows.5 mmol/L borate-25 mmol/L sodium dodecyl sulfate-15% methanol (volume fraction) as the running buffer (pH 9. 2), applied voltage of 25 kV, detection wavelength of 200 nm. Under the optimum conditions, baseline separation of each component in 17 minutes has been obtained using anionic surfactant for micellar electrokinetic chromatography. The detection limits for DMP,DEP,DBP,DEHP and DOP were 0. 13 mg/L,0. 14 mg/L,0.38 mg/L,0. 13 mg/L and 0. 10 mg/L, respectively. The proposed method has been applied to the determination of phthalate esters in food-packaging bags with the recovery in the range of 81. 80% - 118. 87%, the relative standard deviations of peak area(n=10) are less than 4.30 %.
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