加速溶剂萃取-气相色谱测定纺织品中磷酸酯类增塑剂

Determination of Phosphate Ester Plasticizers in Textiles with Accelerated Solvent Extraction(ASE)-Gas Chromatography(GC)

采用加速溶剂萃取结合气相色谱,建立了一种快速提取和测定纺织品中8种磷酸酯类增塑剂(磷酸三苯酯(TPP)、磷酸邻三甲苯酯(ToCP)、磷酸间三甲苯酯(TmCP)、磷酸对三甲苯酯(TpCP)、磷酸三丁酯(TBP)、磷酸三辛酯(TOP)、磷酸二苯辛酯(DPOP)和磷酸甲苯二苯酯(CDP))的分析方法,样品经提取、浓缩,定容,采用HP-5石英毛细管柱(30 m×0.32 mm×0.25μm)分离,火焰光度检测器(FPD)测定,外标法定量。讨论了提取溶剂的选择、方法检测限与线性相关性、方法添加回收率与精密度及气相色谱条件的选择对分析方法的影响。并测试了加入8种磷酸酯类增塑剂的标准溶液的涤纶试样。试验结果表明:在0.1~10.0μg/mL线性关系良好(γ>0.99),在添加浓度为1.0、2.0和5.0 mg/kg时水平内,平均回收率为(93.13±3.12)%^(103.28±4.01)%,相对标准偏差(RSD)为1.74%~5.59%,方法检出限(LOD)为0.90~32.40μg/kg,方法定量限(LOQ)为2.97~106.92μg/kg。该方法操作简便、快捷、灵敏、准确,适合纺织品中8种磷酸酯类增塑剂的确证和定量测定。

This study uses accelerated solvent extraction in combination with gas chromatography to establish an analysis method for rapid extraction and determination of eight phosphate ester plasticizers （Triphenyl Phosphate （ TPP）, Tricresy Phosphate （ ToCP）, Cresyl Phosphate （ TmCP）, Tri-o-cresyl Phosphate （ TpCP）, Tributyl Phosphate （TBP）, Trioctyl Phosphate （ TOP）, Diphenyl Octylphosphate （DPOP） and Diphenyl Tolyl Phosphate （CDP） ） in textiles. Samples are separated by using HP-5 fused silica capillary column （30 m × 0.32 mm× 0. 25 μm） after extraction, concentration and constant volume, determined by using flame photometric detector（FPD） and quantified with external standard method. This paper discusses the influence of selection of extraction solvent, method detection limit and linear dependence, method added recovery, degree of precision and selection of GC conditions and tests polyester samples of standard solution with 8 phosphate ester plasticizers. The test result shows that： the linear relation is good（γ 〉0.99） within the scope of 0. 1 -10.0 μg/mL; when additive concentration is 1.0, 2.0 and 5.0 mg/kg, the average recovery rate scope is （93. 13 ± 3. 12 ） % - （ 103.28 ± 4.01 ） % , relative standard deviation（RSD） is i. 74% -5.59% , limit of detection（LOD） is 0.90 - 32.40 μg/kg and limit of quantitation （LOQ） is 2.97 - 106.92 μg/kg. This method is easy to operate, rapid and convenient, sensitive and accurate and is appropriate for the confirmation and quantitative determination of eight phosphate ester plasticizers in textiles.