液相色谱-串联质谱法快速测定食品中的可乐定

Rapid determination of clonidine in food by liquid chromatography-electrospray tandem mass spectrometry

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 develop a rapid method for determination of clonidine in foodstuffs by liquid chromatography tandem mass spectrometry(LC-MS/MS) and provide analytical methodology for the relevant food poison accidents.Methods Homogenized samples were ultrasonically extracted by methanol-water solution,separated on a Waters ACQUITY UPLCTM BEH C18 column with gradient elution using methanol and water containing 0.1% formic acid at a flow rate of 0.3 mL/min and analyzed by LC-MS/MS.Mass data acquisition was conducted under the positive ion mode with multi-reaction monitoring(MRM).Results Average recoveries of clonidine fortified in fried chicken and starch samples at three spiked levels were 91.5%～127.8% with relative standard deviations less than 16.0%.The limit of quantitation(LOQ) for the whole method was 20 μg/kg.Conclusion Due to its simplicity,high sensitivity and reproducibility,the method is suitable for the detection of clonidine in foodstuffs.It has been applied to analyze the target compound in the real food samples collected from the Huairou Shanba hotel in April 2010.