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作 者:李贞[1]
出 处:《分析试验室》2016年第10期1152-1156,共5页Chinese Journal of Analysis Laboratory
基 金:内蒙古自治区高等学校科学研究项目(NJZC13407);内蒙古商贸职业学院课题项目(NSZY1113)资助
摘 要:建立了气相色谱-质谱法(GC-MS)同时测定木质食品接触材料中10种多氯苯酚化合物含量的检测方法。样品中10种多氯苯酚化合物经甲醇萃取,提取液在K_2CO_3溶液环境中经乙酸酐乙酰化后以正己烷萃取,经DB-5MS型毛细管气相色谱柱分离,质谱定量。结果表明:10种多氯苯酚化合物含量在1.0~200μg/m L范围内呈良好的线性关系,线性相关系数R^2>0.9996;检出限均低于1.0 mg/kg;回收率为88.4%~103.6%,相对标准偏差(n=6)为2.1%~4.6%。方法能够满足对木质食品接触材料中10种多氯苯酚化合物的分析要求。An analytical method using gas chromatography-mass spectrometry( GC-MS) was established for simultaneous determination of 10 kinds of chlorinated phenols in wooden food contact material. 10 kinds of chlorinated phenols in samples were extracted by methanol,and acetylized by acetic anhydride in potassium carbonate solution with n-hexane extraction after acetylation. The extracts were purified by sulfuric acid,and condensed and dissolved in fixed volume,and separated by DB-5MS glass capillary column,and quantified by mass spectrometry. The results showed that the calibration curves for 10 kinds of chlorinated phenols were linear in the range of 1. 0 ~ 200 μg/m L,and the linearly dependent coefficient( R^2) were higher than 0. 9996; the detection limits were less than 1. 0 mg/kg; the mean recoveries of 10 kinds of chlorinated phenols were 88. 4%~ 103. 6%; the relative standard deviation( n = 6) were 2. 1% ~ 4. 6%. The method can be applied to determination of chlorinated phenols in wooden food contact material by gas chromatography-mass spectrometry with easy operation,high recovery,high precision,and low detection limit.
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