超高效液相色谱-串联质谱法检测生肉中的阿托品和山莨菪碱

Determination of anisodamine and atropine in raw meat by ultra performance liquid chromatography-tandem mass spectrometry

目的建立超高效液相色谱串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)同时检测生肉中的阿托品和山莨菪碱的残留量。方法生肉样品加水均质后经乙腈超声提取,采用正己烷除油,旋干后定容上机检测。实验中采用了Agilent Eclipse Plus C_18色谱柱,以0.1%甲酸水溶液-甲醇为流动相,进行梯度洗脱,流速为0.3 m L/min,柱温40℃。结果阿托品和山莨菪碱在0.5~20 ng/m L的质量浓度范围内线性关系良好,相关系数均在0.999以上。分别对其进行1.0、5.0、10 ng/m L不同浓度的加标实验,回收率介于70.77%~89.09%。阿托品和山莨菪碱的方法检出限分别为0.056、0.025μg/kg,定量限分别为0.072、0.030μg/kg。结论该实验方法简单、快速,回收率较好,方法检出限较低,适用于快速检测生肉样品中阿托品和山莨菪碱的残留量。

Objective To establish a method for detection of anisodamine and atropine residues in raw meat by ultra performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. Methods The samples of raw meat were extracted with acetonitrile under ultrasonic, and grease were removed by hexane. The obtained solution was concentrated by vacuum-rotary evaporation, and then dissolved for detection. Gradient elution was conducted on Agilent Eclipse Plus C_18 column. The gradient elution was performed with 0.1% formic acid solution-methanol as liquid phase, and the flow rate of 0.3 m L/min, column temperature 40 ℃. Results This method had high sensitivity and good linear correlation from 0.5 to 20 ng/m L with all correlation coefficient above 0.999. The average recoveries were in the range of 70.77%~89.09% at spiked levels of 1.0, 5.0 and 10 ng/m L. The limits of detection of atropine and anisodamine were 0.056, 0.025 μg/kg, respectively. The limit of quantification were 0.072, 0.030 μg/kg, respectively. Conclusion The method is simple and rapid with good recovery and low limit of detection, which can meet the rapid test of the residue of atropine and scopolamine in raw meat.