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目的建立腐竹、米线、年糕中乌洛托品的超高压液相色谱-串联质谱分析方法。方法样品经粉碎后,用乙腈提取,MCX小柱净化,Waters ACQUITYTM UPLC BEH HILIC色谱柱分离,最后在电喷雾正离子多反应监测模式下,用超高压液相色谱-串联质谱仪进行分析。结果乌洛托品在1.00～100.00μg/L的范围内呈现良好的线性关系良好,线性方程为Y=2391.11X+253.197,R2大于0.99。该方法检出限(S/N=3)和定量限(S/N=10)分别为0.30μg/kg和1.00μg/kg。在1.00、10.00、50.00μg/kg三个添加水平下,乌洛托品平均回收率为82.0%～107.0%,相对标准偏差为6.3%～15.6%。结论该方法操作简便、检出限低,能够满足腐竹、米线、年糕中乌洛托品检测的要求。
Objective To establish a method for the determination of urotropine in bean curd, rice noodle and rice cake by ultra high pressure liquid chromatography-tandem mass spectrometry. Methods After the sample was crushed, it was extracted with acetonitrile, purified by MCX cartridge, and separated on a Waters ACQUITY UPLC BEH HILIC column. Finally, the data were analyzed by EHPLC-tandem mass spectrometry in the electrospray positive ionization multiple reaction monitoring mode. Results Urotropine showed a good linearity in the range of 1.00-100.00μg / L with linear equation Y = 2391.11X + 253.197 and R2 greater than 0.99. The method detection limit (S / N = 3) and the limit of quantification (S / N = 10) were 0.30μg / kg and 1.00μg / kg respectively. The average recoveries of urotropin ranged from 82.0% to 107.0% and the relative standard deviations (RSDs) ranged from 6.3% to 15.6% at three levels of 1.00, 1.00 and 50.00 μg / kg. Conclusion The method is simple, low detection limit, and can meet the requirements of urotropine detection in yuba, rice noodle and rice cakes.