固相萃取-气相色谱-串联质谱内标法测定一次性食品用纸制品中五氯酚残留  

Determination of residual pentachlorophenol in disposable paper products for food by solid phase extraction-gas chromatography-tandem mass spectrometry internal standard method

作　　者：杨长晓[1] 张坤[1] 钟海洋 YANG Chang-xiao;ZHANG Kun;ZHONG Hai-yang(Sichuan Center for Disease Control and Prevention,Chengdu,Sichuan 610041,China)

机构地区：[1]四川省疾病预防控制中心,四川成都610041 [2]凉山彝族自治州疾病预防控制中心

出　　处：《现代预防医学》2021年第1期144-147,共4页Modern Preventive Medicine

摘　　要：目的建立一次性食品用纸制品中五氯酚残留的固相萃取-气相色谱-串联质谱测定方法。方法样品粉碎后,加入2,4,6-三溴苯酚内标,酸性条件下用乙酸乙酯-正己烷混合溶剂(2:8,v/v)提取,SLC固相萃取柱净化,乙酸酐-吡啶溶液衍生,内标和目标物分别转化成2,4,6-三溴苯乙酸酯和五氯苯乙酸酯。用正己烷提取,气相色谱-串联质谱法分析,内标法定量。结果在10~500 ng范围内,五氯酚具有良好的线性关系(r=0.9998),检出限为0.01 mg/kg,定量限为0.03 mg/kg。平均加标回收率为93.6%~104.6%,相对标准偏差(RSD)为3.6%~8.2%(n=6)。结论本方法具有准确性高、灵敏度高、快速等特点,适用于一次性食品用纸制品中五氯酚的定量测定。Objective To establish a solid phase extraction-gas chromatography-tandem mass spectrometry method for determining residual pentachlorophenol in disposable paper products for food.Methods After the sample was pulverized,2,4,6-tribromophenol as the internal standard was added,followed by extraction using ethyl acetate-n-hexane(2:8,v/v)mixed solvent under an acid condition and purification using SLC solid phase extraction cartridges.An acetic anhydride-pyridine solution was added to transform the internal standard and the analyte into 2,4,6-tribromophenyl acetate and pentachlorophenyl acetate,respectively.The derivatives were extracted with n-hexane andanalyzed by gas chromatography-tandem mass spectrometry.The quantification was based onthe internal standard method.Results Good linearity was obtained over a range of 10-500 ng(r=0.9998).The limit of detection was 0.01 mg/kg;and the limit of quantitation was 0.03 mg/kg.The average recovery was 93.6%-104.6%,with the relative standard deviations(RSD)of 3.6%-8.2%(n=6).Conclusion The established method is sensitive,rapid and accurate and is suitable for determination of pentachlorophenol in disposable paper products for food.

关 键 词：食品用纸制品 气相色谱-串联质谱法 五氯酚 固相萃取 内标法 

分 类 号：R155.5[医药卫生—营养与食品卫生学]