同位素稀释-气相色谱三重四极杆质谱法测定水性内墙涂料中的苯酚与氯代苯酚防霉杀菌剂

Determination of phenol and chlorophenols in interior latex paint by lsotope Dilution-GC-MS / MS

建立了同位素稀释-气相色谱串联三重四极杆质谱（GC-MS/MS）测定水性内墙涂料中苯酚及氯代苯酚（2-氯苯酚、2,4-二氯苯酚、2,4,6-三氯苯酚、2,3,4,6-四氯苯酚、五氯苯酚、邻苯基苯酚和六氯芬）防霉杀菌剂的方法。样品加入同位素内标,经甲醇超声提取,乙酸酐衍生后正己烷提取,采用GC-MS/MS测定,内标法定量,方法检出限均为0.005 mg/kg。目标物在0.02～1 mg/kg范围内线性良好,相关系数大于0.99,添加回收率为75.3%～107.6%,相对标准偏差为4.3%～14%。方法可以满足以丙烯酸、聚醋酸乙烯-丙烯酸和聚苯乙烯-丙烯酸为基材的水性内墙涂料中氯酚类防霉杀菌剂残留的检测要求。

A new method was developed for the determination of phenol and chlorophenols（ 2-chlorophenol,2,4-dichlorophenol,2,4,6-trichlorophenol,2,3,4,6-tetrachlorophenol,pentachlorophenol,o-phenyl-phenol,hexachlorophene） in interior latex paint by isotope dilution-gas chromatography tandem mass spectrometry（ GCMS / MS）. After the addition of isotopic internal standard,the samples were sonicated in methanol,acetylated by acetic anhydride and borate solution,and extracted by hexane,followed by GC-MS / MS analysis. 8 compounds were successfully separated and determined,under the optimized procedure and conditions,with the detection limit of 0. 005 mg / kg. The linear range is 0. 02 mg / kg to 1 mg / kg and the correlation coefficients are higher than 0. 99. This method exhibited a good precision（ 4. 3 % ～ 14%） with recovery of 75. 3 % ～ 107. 6 %. This accurate,rapid and sensitive method can be used to analyze CPs in acrylic polymer,vinyl acetate-acrylic acid copolymer or styrene-acrylic copolymer latex paint.