超高效液相色谱串联质谱法测定腐竹中乌洛托品的含量

Determination of Urotropine in dried beancurd sticks by ultra performance liquid chromatography-tandem mass spectrometry

摘要: 建立用超高效液相色谱-串联质谱法（UPLC-MS/MS）测定腐竹中乌洛托品含量的方法。用乙腈提取腐竹中的乌洛托品,经固相萃取柱PXA净化,用UPLC-MS/MS分析,采用多反应监测模式,外标法定量。采用ACQUITY UPLC BEH HILIC色谱柱,以乙酸铵和乙腈为流动相,进行梯度洗脱。结果表明:该方法标准曲线良好,线性范围为1²0μg/L,最低检出限为1μg/L,三个水平添加浓度的平均回收率范围为81.67%¹01.67%。本方法操作简单快捷,方法准确度和稳定性好。

Abstract: A method for the determination of urotropine in dried beancurd sticks was established by UPLC-MS/MS.The sample was extracted with acetonitrile as extraction solvents, then further purified by PXA solid phase extraction column.The analyte was determined by multi- reaction monitoring ( MRM) mode was employed for the quantitative determination, and quantified by the external standard curve.The separation was performed on a UPLC ACQUITY BEH HILIC column by gradient elution with a system of water ( containing 10 mmol /L ammonium acetate buffer) -acetonitrile as mobile phase.Results showed that the calibration curve had good linearity.The developed method exhibited good linearity over the range from 1 to 20μg /L.The minimum detection limit was 1μg /L. The average recovery rate for urotropine was 81.67% ~ 101.67%.The method is simple, accurate and suitable for the identification and quantification.