在线固相萃取液相色谱-串联质谱法同时测定食品中的敌敌畏和敌百虫

Simultaneous determination of dichlorvos and trichlorfon in food samples by on-line solid phase extraction liquid chromatography-tandem mass spectrometry

中文关键词:  猪肉  火腿  敌敌畏  敌百虫  在线固相萃取液相色谱-串联质谱法

英文关键词:pork  ham  dichlorvos  trichlorfon  on-line solid phase extraction liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 利用在线固相萃取液相色谱-串联质谱技术建立猪肉、火腿和腊肉中敌敌畏和敌百虫的同时检测方法。方法 样品中的目标化合物经50%乙腈水溶液提取, 上清液用水稀释后经HP XBridgeTM C8柱富集, BEH C18色谱柱分离, 甲醇和水梯度洗脱, 三重四极杆质谱电喷雾正离子模式下采集数据, 基质匹配外标曲线法定量。结果 敌敌畏和敌百虫的线性范围为0.2~50.0 μg/kg, 相关系数r2>0.99; 猪肉、火腿和腊肉中敌敌畏的定量限分别为0.2、0.2和0.5 μg/kg, 敌百虫的定量限分别为0.5、0.5和1.0 μg/kg。3个加标水平的平均回收率为75.6%~104.9%, 相对标准偏差<20%。结论 与已有的检测技术相比, 该方法快速、简单、灵敏度高, 适用于猪肉、火腿和腊肉中敌敌畏和敌百虫的同时检测, 为相关食品中非法添加物的检测提供了技术支持。

英文摘要:

      Objective To establish a method for the simultaneous determination of dichlorvos and trichlorfon in pork, ham and bacon by on-line solid phase extraction liquid chromatography-tandem mass spectrometry. Methods The target compounds in the samples were extracted with 50% acetonitrile water solution, and the supernatant was diluted with water and enriched on an HP XBridgeTM C8 column, the components were separated on a BEH C18 column, and eluted with methanol and water in a gradient manner, the data were collected in a triple quadrupole mass spectrometer electrospray positive ion mode, and quantified by matrix matching external standard curve method. Results The linear ranges of dichlorvos and trichlorfon were 0.2?50.0 μg/kg with the correlation coefficients r2>0.99. The limits of quantification for dichlorvos were 0.2, 0.2 and 0.5 μg/kg for pork, ham and bacon, and 0.5, 0.5 and 1.0 μg/kg for trichlorfon, respectively. The average recoveries at the 3 kinds of spiked levels were 75.6%?104.9% and the relative standard deviations were less than 20%. Conclusion Compared with the existing detection techniques, this method is rapid, simple and sensitive, which is suitable for the simultaneous detection of dichlorvos and trichlorfon in pork, ham and bacon, and provides technical support for the detection of illegal additives in related foods.