快速溶剂萃取-高效液相色谱测定塑料中邻苯二甲酸酯类化合物  被引量:55

Determination of DEHP and DNOP in PVC Film by ASE-RP-HPLC

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作  者:李波平[1] 林勤保[1] 宋欢 李莉莉[1] 

机构地区:[1]山西大学现代化学研究所,太原030006 [2]山西出入境检验检疫局技术中心,太原

出  处:《应用化学》2008年第1期63-66,共4页Chinese Journal of Applied Chemistry

基  金:山西省科技攻关计划资助项目(2007031082)

摘  要:建立了快速溶剂萃取-反相高效液相色谱检测塑料巾邻苯二甲酸二(2-乙基)己基酯(DEHP)和邻苯二甲酸二正辛酯(DNOP)的方法。塑料样品经剪碎后,用二氯甲烷作溶剂经快速溶剂萃取,浓缩、过滤,用反相高效液相色谱Diamond—C18柱(250mm×4.6mm i.d.,5μm)分离,V(乙腈):V(水)=95:5作流动相,流速1.0mL/min;用波长为254nm紫外检测,外标法定量。在DEHP和DNOP的质量浓度为0.1~100mg/L范围内的线性关系良好,相关系数〉0.999。加标回收率87%~108%,RSD〈5.20%。检测限为10mg/L。方法快速、简便易行,分离度较好,可作为测定塑料中增塑剂邻苯二甲酸酯类的方法。A method of accelerated solvent extraction and reverse-phase high performance liquid chromatography(ASE-RP-HPLC) was developed to determine the concentration of phthalates in plastics. The plasticpieces were extracted with dicholoride methane by accelarated solvent extraction (ASE), and then the extractant was concentrated, filtered, and prepared for HPLC analysis. The analysis was performed on a Diamond column (250 mm ×4.6 mm i. d. , 5 μm) with acetonitrile-water(95:5, volume ratio) as the mobile phase at a flow rate of 1.0 mL/min, and it was detected at 254 nm using a UV detector. Quantitative analysis was carried out with external standard method. The calibration curves were linear in the range of 0. 1~100 mg/L and the correlation coefficients were above 0. 999 for both compounds. The relative standard deviations were below 5.20%. The recoveries of both phthalates added were 87% ~ 108%. The detection limit of the method was 10 mg/L. The method is a fast and simple one to detect the concentration of phthalates in plastics.

关 键 词:反相高效液相色谱 快速溶剂萃取 邻苯二甲酸二(乙基)己基酯 邻苯二甲酸二正辛酯 

分 类 号:O655[理学—分析化学]

 

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