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

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。

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

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.