QuEChERS-混合型吸附剂分散固相萃取-气相色谱-三重四级杆串联质谱法测定鸡肉和猪肉中的五氯酚

目的 建立QuEChERS-混合型吸附剂分散固相萃取-气相色谱-三重四级杆串联质谱法(gas chromatography-triple quadrupole mass spectrometry,GC-MS/MS)测定鸡肉和猪肉中五氯酚的方法。 方法 样品用5%的三氯乙酸沉淀蛋白质,加入乙腈和QuEChERS萃取包提取,混合型吸附剂进行分散固相萃取净化,乙酸酐-吡啶溶液衍生。GC-MS/MS测定,以2,4,6-三溴酚为内标定量。 结果 本实验测定的五氯酚具有良好的线性关系(r＞0.999),检出限(S/n=3)为0.01 μg/kg,定量限为0.03 μg/kg,回收率为89.8%～115.2%,相对标准偏差为1.6%～11.3%。 结论 该方法操作简单,定量准确,重现性和精密度良好,检出限较低,适用于鸡肉和猪肉中五氯酚的检测。

Determination of pentachlorophenol in chicken and pork by QuEChERS-mixed adsorbent dispersive solid phase extraction with gas chromatography-triple quadrupole mass spectrometry

Objective To establish a method for the determination of pentachlorophenol in chicken and pork usingQuEChERS-mixed adsorbent dispersive solid phase extraction with gas chromatography-triple quadrupole mass spectrometry (GC-MS/MS). Methods Five percent trichloroacetic acid was added to samples to precipitate proteins, then acetonitrile and QuEChERS extraction package were added to extract. Mixed adsorbents were used to disperse solid phase extraction andpurification, and derived with acetic anhydride pyridine solution. GC-MS/MS was applied to determination, and2,4,6-tribromophenol was selected as internal standard for quantification. Results The pentachlorophenol measured in this experiment had a good linear relationship (r>0.999). The limit of detection (S/n=3) was 0.01μg/kg, and the limit of quantification 0.03μg/kg. The recoveries ranged from 89.8% to 115.2%, and the relative standard deviation from 1.6% to 11.3%. Conclusion The method is simple in operation, accurate in quantification, good in reproducibility and precision, and of low detection limit. It is suitable for the detection of pentachlorophenol in chicken and pork.