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利用液相串联质谱法测定食品中乌洛托品。样品经乙腈提取、正己烷除脂,Oasis MCX固相萃取柱净化,以乙腈-10mmol/L乙酸铵溶液为流动相,超高效液相色谱-串联质谱仪进行分析。结果表明:在0~100μg/L,乌洛托品所得的回归方程呈良好的线性关系,相关系数大于0.999。该方法检出限(S/N=3)和定量限(S/N=10)分别为0.3和1.0μg/kg。该方法的平均回收率为86.2%~94.2%,RSD为1.67%~3.06%。该方法快速、准确和灵敏,适用于食品中乌洛托品的测定及确认。
Determination of Urotropine in Food by Liquid Chromatography - Tandem Mass Spectrometry. Samples were extracted with acetonitrile, hexane was degreased and purified by Oasis MCX SPE cartridge. The mobile phase was acetonitrile-10 mmol / L ammonium acetate solution and analyzed by ultra performance liquid chromatography-tandem mass spectrometry. The results showed that there was a good linear relationship between the regression equation of urotropine and 0 ~ 100 μg / L with the correlation coefficient greater than 0.999. The method detection limit (S / N = 3) and the limit of quantification (S / N = 10) were 0.3 and 1.0μg / kg. The average recoveries of this method ranged from 86.2% to 94.2% with RSDs ranging from 1.67% to 3.06%. The method is rapid, accurate and sensitive and is suitable for the determination and confirmation of urotropine in food.