摘要
建立了橡胶及其制品中硝基苯酚（PNP）、2，3，5，6-四氯苯酚（TeCP）、五氯苯酚（PCP）、邻苯基苯酚（OPP）4种酚类防腐剂的高效液相色谱测定方法。样品冷冻粉碎后，经甲醇超声提取，在Venusil—XBPC18色谱柱（250mm×4．6mm，5μm）上以10mmol／L醋酸铵和甲醇为流动相梯度洗脱，采用二极管阵列检测器，PCP、TeCP、OPP的检测波长为220nm，PNP的检测波长为320nm。4种酚类防霉剂的质量浓度在0．5～250mg／L范围内与峰面积呈良好的线性关系，相关系数大于0．9994。丁苯橡胶、硅橡胶基体的加标回收实验结果表明：TeCP、PCP、OPP、PNP在不同基质中的平均加标回收率分别为82％一95％、68％一90％、8596—98％、87％一98％，相对标准偏差小于5％。
A high performance liquid chromatographic （HPLC） method was developed for the determination of four phenolic antiseptics, including nitrophenol （PNP）, 2, 3, 5, 6-tetrachlorophenol （ TeCP）, pentachlorophenol（ PCP）, o-phenylphenol（OPP） in rubber and rubber products. After freeze grinding, the samples were ultrasonicly extracted with methanol. The separation and quantification of four phenolic antiseptics were achieved by an Venusil-XBP C18（250mm ×4.6mm,5μm） using a mixture of 10 mmol/L NH4Ac and methanol as the mobile phase and detecting with diode array detector （DAD） at 220 nm for PCP, TeCP, OPP, and 320 nm for PNP. There were good linear relationship between the chromatographic peak areas and the concentrations of four phenolic antiseptics in the range of 0. 5 - 250 mg/L with correlation coefficients more than 0. 999 4. The recoveries of spiked samples in different matrix were 82% -95% for TeCP, 68% -90% for PCP, 85% -98% for OPP and 87% - 98% for PNP, respectively. The relative standard deviations （ n = 6 ） were lower than 5% . The results showed that the method was simple, rapid and accurate, and was successfully applied in the analysis of phenolic antiseptics in rubber and rubber products.
出处
《分析测试学报》
CAS
CSCD
北大核心
2010年第3期226-231,共6页
Journal of Instrumental Analysis
基金
国家质检公益性行业科研专项基金资助项目(10-66)
关键词
酚类防腐剂
橡胶
硝基苯酚
2
3
5
6-四氯苯酚
五氯苯酚
邻苯基苯酚
高效液相色谱
phenolic antiseptics
rubber
nitrophenol
2, 3, 5, 6-tetrachloro-phenol
pentachlorophenol
o-phenylphenol
high performance liquid chromatography（HPLC）
