高效液相色谱法测定合成橡胶材料中两种胍类硫化促进剂残留量的研究 |
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中文摘要:建立了一种快速测定合成橡胶材料中1,3 二苯胍(DPG)和1,3 二邻甲苯胍(DOTG)2种胍类硫化促进剂残留量的高效液相色谱法(HPLC)。样品以甲醇作溶剂经索氏抽提后,以C18色谱柱分离,乙腈和磷酸缓冲盐为流动相进行梯度洗脱,紫外检测波长为235 nm,外标法定量。该方法中DPG和DOTG在2~50 mg/L质量浓度范围内呈良好的线性关系,相关系数均为0999 9,方法检出限分别为30 mg/kg和40 mg/kg。在10、20、40 mg/L加标水平下,样品的平均加标回收率为824%~945%,相对标准偏差(RSD,n=5)为10%~33%。该方法简单、快速、可靠性高,适用于合成橡胶材料中DPG和DOTG残留量的测定。 |
中文关键词:橡胶材料 硫化促进剂 胍 高效液相色谱法 |
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Determination of Two Kinds of Guanidines Vulcanization Accelerator Residues in Synthetic Rubber Materials by High Performance Liquid Chromatography |
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Abstract:A new method was established for the determination of two kinds of guanidines vulcanization accelerators,1,3 diphenyl guanidine(DPG) and 1,3 di o tolylguanidine(DOTG) in synthetic rubber materials by high performance liquid chromatography(HPLC).The samples were extracted by soxhlet extraction with methanol,and separated on a C18 column with acetonitrile-phosphate buffer as mobile phase by gradient elution.The UV detection wavelength was set at 235 nm,and the external standard method was used for quantitative analysis.There were good linear relationships for the two componds in the concentration range of 2-50 mg/L with their correlation coefficients both 0999 9.The limits of detection of the method(MLODs) were 30 mg/kg and 40 mg/kg,respectively.The average recoveries for the analytes were in the range of 824%-945%,with the relative standard deviations(RSD,n=5) of 10%-33%.This method was simple,rapid and reliable,and was suitable for the determination of DPG and DOTG residues in synthetic rubber materials. |
Key Words:rubber material vulcanization accelerator guanidine high performance liquid hromatography(HPLC) |
引用本文:余国枢,区棋铭,黄雨锟,叶志武.高效液相色谱法测定合成橡胶材料中两种胍类硫化促进剂残留量的研究[J].分析测试学报,2018,37(7):830-833. |
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