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目的建立腐竹中乌洛托品的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。方法样品经乙腈/水(1:1,v:v)溶液超声提取,阳离子交换柱净化后,经Waters Acquity UPLC BEH HILIC(2.1 mm×100 mm,1.7μm)色谱柱分离,在电喷雾正离子多反应监测模式下进行测定。结果乌洛托品在0.5~100.0μg/L范围内线性关系良好,相关系数(r)大于0.999。方法检出限和定量限分别为6μg/kg和20μg/kg。在20、40、100μg/kg 3个空白加标水平下,乌洛托品的加标回收率为100.1%~103.9%,相对标准偏差为4.7%~8.9%。结论该方法快速、简便、准确可靠,适用于腐竹中非法添加的乌洛托品的含量测定。
Objective To establish a method for the determination of urotropine in yuba by UPLC-MS / MS. Methods The samples were extracted with acetonitrile / water (1: 1, v: v) by sonication and purified by cation exchange column. The samples were separated on Waters Acquity UPLC BEH HILIC (2.1 mm × 100 mm, 1.7 μm) Multiple reaction monitoring mode for the determination. Results Urotropin showed a good linearity in the range of 0.5-100.0 μg / L with a correlation coefficient (r) greater than 0.999. The detection limits and the limits of quantitation were 6μg / kg and 20μg / kg, respectively. The spiked recoveries of urotropine ranged from 100.1% to 103.9% at 3 spiked levels of 20, 40 and 100 μg / kg, with relative standard deviations of 4.7% -8.9%. Conclusion The method is rapid, simple, accurate and reliable and is suitable for the determination of urotropine illegally added in yuba.