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目的采用超高压液相色谱-电喷雾串连四极杆质谱分析食品基质中的可乐定,为可乐定中毒事件的样本分析提供依据。方法食物样本粉碎后经甲醇水溶液超声提取,低温离心后,上清液用Waters ACQUITYUPLCTM BEH C18色谱柱分离,以0.1%甲酸和甲醇溶液为流动相梯度洗脱,最后用串联四极杆质谱在正离子MRM模式下进行测定。结果以淀粉和炸鸡为加标基质,三个加标水平下可乐定的平均回收率为91.5%～127.8%,相对标准偏差小于16%,定量限为0.02 mg/kg。结论该方法操作快速简单、重现性好,成功用于2010年4月怀柔水岸山吧可乐定中毒事件的食品检测。
Objective To analyze the clonidine in food matrix by ultra-high pressure liquid chromatography-electrospray tandem quadrupole mass spectrometry (MS-MS / MS), providing the basis for sample analysis of clonidine poisoning. Methods After the food sample was crushed, it was extracted with methanol aqueous solution. After centrifugation at low temperature, the supernatant was separated on a Waters ACQUITY UPLC BEH C18 column. The mobile phase was eluted with 0.1% formic acid and methanol. The final concentration was determined by tandem quadrupole mass spectrometry Ion MRM mode determination. Results The average recoveries of clonidine at three spiked levels were 91.5% -127.8% with relative standard deviations less than 16%. The limit of quantification was 0.02 mg / kg. Conclusion The method is rapid, simple and reproducible. It is successfully applied to the food testing of clonidine poisoning in Huairou Waterfront Hill in April 2010.