离子交换固相萃取-超高效液相色谱-串联质谱法 快速测定腐竹中的乌洛托品

Rapid determination of urotropine in dried beancurd sticks by ultra-performance liquid chromatography-tandem mass spectrometry coupled with ion exchange solid phase extraction

中文关键词:  乌洛托品  腐竹  超高效液相色谱-串联三重四级杆质谱法  离子交换固相萃取法

英文关键词:urotropine  dried beancurd sticks  ultra-performance liquid chromatography-tandem mass spectrometry  ion exchange solid phase extraction

中文摘要:

      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, 1.7 μm)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. 5~100.0 μg/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6 μg/kg和20 μg/kg。在20、40、100 μg/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。

英文摘要:

      Objective To establish a method for the determination of urotropine in dried beancurd sticks by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples were ultrasonically extracted by acetonitrile/water (1:1, v:v), and then purified by cation exchange solid phase extraction. The analytes were separated on a Waters Acquity UPLC BEH HILIC column (2.1 mm × 100 mm, 1.7 μm) and detected by positive electrospray ionization in multiple reactions monitoring (MRM). Results The method showed a good linearity over the range of 0.5~100.0 μg/L with relative coefficient not less than 0.999. The limit of detection (LOD) and the limit of quantification (LOQ) were 6 μg/kg and 20 μg/kg, respectively. The average recoveries of urotropine at the spiking levels of 20, 40 and 100 μg/kg were in the range of 100.1%~103.9%, with the relative standard deviations in the range of 4.7%~8.9%. Conclusion The method is rapid, simple and accurate for the determination of urotropine in dried beancurd sticks.