2-乙烯基吡啶中对叔丁基邻苯二酚分析方法的建立

Establishment Method on the Determination of 4-tert-Butylcatechol in 2-vinylpyridine

目的:建立测定2-乙烯基吡啶中对叔丁基邻苯二酚含量的高效液相色谱法。方法:采用十八烷基硅烷键合硅胶为填充剂,取十二烷基硫酸钠2.0 g,溶于10%(v/v)硫酸溶液15 mL,17 g·L^(-1)四丁基硫酸氢铵35 mL和水650 mL的混合液中,用氢氧化钠试液调节pH值至3.3,然后与300 mL乙腈混合均匀,作为流动相;检测波长为280 nm,柱温为30℃,流速1 mL·min^(-1),进样量为10μL。结果:溶剂不干扰测定,在0.2046~4.092μg·mL^(-1)浓度范围内线性良好,重复性良好,检测限为0.170μg·mL^(-1),定量限为0.512μg·mL^(-1),低、中、高3个浓度的平均回收率为91.80%,RSD为2.4%。结论:该方法简便、准确、灵敏度高、重现性好,适用于2-乙烯基吡啶中对叔丁基邻苯二酚的检查。

Objective:To establish a HPLC method for the determination of 4-tert-Butylcatechol in 2-Vinylpyridine.Methods:The 4-tert-Butylcatechol was separated on a base-deactivated end-capped octadecylsilyl silica gel chromatographic column.Dissolve 2.0 g of sodium dodecyl sulfate in a mixture of 15 mL of a 10 per sent V/V solution of sulfuric acid,35 mL of a 17 g·L^(-1) solution of tetrabutylammonium hydrogen sulfate and 650 mL of water as the mobile phase,the spectrophotometer was 260 nm,the temperature of column was 30℃,the flow rate was 1 mL min^(-1),and the injection was 10μL.Results:Determination was not interfered by the solvent.Over a concentration range of 0.2046μg·mL^(-1) to 4.092μg·mL^(-1),it displayed a good linear relationship(R=0.9995).The LOD and LOQ of 4-tert-Butylcatechol in 2-Vinylpyridine was 0.170μg·mL^(-1) and 0.512μg·mL^(-1) respectively.The average recovery rate of 4-tert-Butylcatechol was 91.80%(RSD=2.4%).Conclusion:The established method was specific,accurate and convenient,which can be used for the determination of 4-tert-Butylcatechol in 2-Vinylpyridine.