稳定性同位素稀释-超高效液相色谱串联质谱法测定腐竹中的乌洛托品

徐幸; 张晓鸣; 张燕; 舒平; 彭飞进

doi:10.13386/j.issn1002-0306.2015.15.050

稳定性同位素稀释-超高效液相色谱串联质谱法测定腐竹中的乌洛托品

徐幸^1,2,
张晓鸣¹,
张燕²,
舒平²,
彭飞进²

1. 江南大学食品学院
2. 大理州质量技术监督综合检测中心

基金项目:

云南省卫生厅制修订食品安全地方标准项目(云卫[2014]DB004)；

详细信息

作者简介:
徐幸(1983-),女,在读博士,工程师,研究方向:食品安全质量检测,E-mail:amy911007@163.com。;

张晓鸣(1965-),男,博士,教授,研究方向:食品安全质量控制,E-mail:xmzhang@jiangnan.edu.cn。;

中图分类号: O657.63;TS214.2
计量
- 文章访问数: 154
- HTML全文浏览量: 27
- PDF下载量: 104
出版历程
- 收稿日期: 2014-11-12

Determination of urotropine in bean curd sticks by stable isotopic dilution- liquid chromatography with tandem mass spectrometry

School of Food Science and Technology,Jiangnan University
Dali Comprehensive Inspection Centre of Quality and Technical Supervision

摘要

摘要: 采用超高效液相色谱-串联质谱法（UPLC-MS/MS）和稳定性同位素稀释技术,建立了测定腐竹中乌洛托品的分析方法。以乙腈为提取溶剂,向腐竹样品中加入乌洛托品的稳定性同位素,经固相萃取柱净化,采用HILIC色谱柱分离,目标物在UPLC-MS/MS的多反应监测（MRM）模式下,内标法定量。该方法在1⁴0μg/L范围内有良好的线性关系,相关系数为0.9996,方法定量限为2μg/kg。在添加水平为2、10、30μg/kg时,平均回收率为97.8%¹01.5%,相对标准偏差（RSD）为1.9%⁴.8%。本方法灵敏度高,准确度和重复性好,可为作为检测腐竹中违法添加乌洛托品的方法。
- 稳定性同位素稀释技术 /
- 超高效液相色谱-串联质谱法 /
- 乌洛托品 /
- 腐竹
Abstract: A stable isotope dilution mass spectrometry technology for determination of urotropine in bean curd sticks by liquid chromatography with tandem mass spectrometry was developed.Isotopic urotropine was added to bean curd sticks as internal standard,and extracted with acetonitrile.Solid phase extraction( SPE) was applied to purify the sample.The separation was performed on a HILIC column. The analyte was determined by multiple reaction monitoring( MRM) mode with UPLC- MS / MS,and quantified by the internal standard method.The method showed good linear relationship in the range of 1⁴0 μg / L for urotropine,the correlation coefficient square was 0.9996.The limit of quantitation( LOQ) for sample was 2 μg / kg.The average recoveries were 97.8% ¹01.5% at spiked levels of2,10,30 μg / kg.The relative standard deviation( RSD,n = 6) was 1.9% ⁴.8%.This method is sensitive,accurate and reproducible.It is suitable for monitoring illegally added urotropine in bean curd sticks.
- stable isotope dilution technology /
- ultra performance liquid chromatography-tandem mass spectrometry /
- urotropine /
- bean curd sticks

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参考文献(15)

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