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。
-
关键词:
- 超高效液相色谱-串联质谱法 /
- 腐竹 /
- 乌洛托品 /
- 检测
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. -
[1] SN/T 2226-2008进出口动物源性食品中乌洛托品残留量的检测方法液相色谱-质谱/质谱法[S]. [2] 张涛, 李战海, 李炎, 等.非法食品添加剂乌洛托品的拉曼光谱及DFT分析方法[J].检验检疫学刊, 2013 (2) :36-37. [3] 李薇, 陈天科, 徐辉, 等.乌洛托品的气相色谱分析[J].分析仪器, 2007 (3) :29-31. [4] 黄国春.气相色谱法测定腐竹中乌洛托品含量的研究[J].广西轻工业, 2008 (6) :26-27. [5] 李莉, 张钢平.高效液相色谱法测定乌洛托品片的含量[J].中国医院药学杂志, 2009 (4) :335-336. [6] 洗燕萍, 陈立伟, 罗东辉, 等.UPLC-MS/MS测定腐竹和米粉中的乌洛托品[J].江南大学学报:自然科学版, 2012, (11) :78-82. [7] 陆春良, 刘娟, 刘向农.亲水作用液相色谱电喷雾串联质谱法测定米线中乌洛托品残留[J].扬州大学学报:农业与生命科学版, 2013 (2) :82-86.
计量
- 文章访问数:
- HTML全文浏览量:
- PDF下载量:
下载:
