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    高效液相色谱法测定烟用白乳胶中邻苯二甲酸酯类化合物

    HPLC Determination of Phthalates in Polyvinyl Emulsion Adhesive Used for Cigarette

    • 摘要: 采用高效液相色谱法测定卷烟用白乳胶中7种邻苯二甲酸类化合物(PAE′s),即邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二异丁酯(DIBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)和邻苯二甲酸二正辛酯(DNOP)。样品用乙腈超声提取,分取部分上清液,经0.45 μm滤膜过滤后,用Zorbax Eclipse XDB-C18色谱柱为固定相,不同比例混合的乙腈和水作流动相进行梯度洗脱,用二极管阵列检测器在波长254 nm处检测。上述7种PAE′s的峰面积与其质量浓度均在1~100 mg·L-1范围内呈线性关系,检出限(3s)在2.7~4.4 mg·kg-1之间。加入3个浓度水平的混合标准溶液做回收试验,测得其回收率在77.9%~114%之间,测定值的相对标准偏差(n=5)在1.6%~8.1%之间。

       

      Abstract: HPLC was applied to the simultaneous determination of 7 phthalates (PAE′s) in polyvinyl emulsion adhesive used for cigarette, i.e., dimethyl phthalate (DMP), diethyl phthalate (DEP), dibutyl phthalate (DBP), di-isobutyl phthalate (DIBP), benzylbutyl phthalate (BBP), bis (2-ehylhexyl) phthalate(DEHP) and dinoctyl phthalate (DNOP). The sample was extracted ultrasonically with acetonitrile, an aliquot of the extract was filtered and separated on Zorbax Eclipse XDB-C18 chromatographic column with mixtures of acetonitrile and water in different ratios as mobile phases in gradient elution. The contents of the 7 PAE′s were determined by DAD-detector at the wavelength of 254 nm. Linear relationships between values of peak area and mass concentration of the 7 PAE′s were kept in the same range of 1-100 mg·L-1, with limits of detection (3s) in the range of 2.7-4.4 mg·kg-1. Tests for recovery were made by addition of mixed standard solution at 3 different concentration levels, values of recovery found were in the range of 77.9%-114% with RSD′s (n=5) in the range of 1.6%-8.1%.

       

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