摘要
以2,4，6-三氯苯酚为内标，建立了纸质材料中五氯苯酚残留量的气相色谱／质谱联用（GC／MS）测定方法。0．5g纸质材料样品以乙醇为萃取溶剂，超声提取30min，提取液经浓缩后用碳酸钾水溶液溶解，经乙酸酐乙酰化后以正己烷提取，以HP．5MS色谱柱分离，采用选择离子扫描（SIM）方式对五氯苯酚进行了测定，内标法定量。实验结果表明，五氯苯酚缌陛关系良好（R2〉0．9999），在3种浓度（0．105μg、0．315μg和0．525μg）的加标水平下，回收率为85．0％～98．1％，相对偏差小于6％，方法的检出限为0．02mg／kg，定量限为0．07mg／kg。方法的样品前处理过程简单，易操作，适用于纸质材料中五氯苯酚残留量的检测。
A rapid analytical method for the determination of pentachlorophenol （PCP） residual in paper materials with 2, 4, 6-trichlomphenol as the internal standard was developed. The paper material was extracted ultrasonically using ethanol in 30 minutes. The concentrated PCP extract was dissolved by 0.1 mol/L potassium carbonate solution, followed by derivation with acetic anhydride. The derivative was extract by n-hexane, and then analyzed in gas chromatography-mass spectrometry （CJC/MS）. The separation was performed on a HP-5MS column （30 m×0.25 mm, 0.25 m film thickness）. The limits of detection （LOD） and limits of quantitation （LOQ） of PCP in the method were 0.02 mg/kg and 0.07 mg/kg by calculating the diluted standard mixture with the 0.5 g of sample matrix, and the recovery was 85.0% ～98.1% with relative standard deviation （RSD） less than 6%. The study revealed that the method was suitable for the determination of residual pentachlomphenol in paper materials.
出处
《现代食品科技》
EI
CAS
北大核心
2012年第12期1818-1821,共4页
Modern Food Science and Technology
