在线SPE液质联用法分析原料糖浆中2-氨基乙酰苯

陈盛; 金燕; 刘绿叶

doi:10.13386/j.issn1002-0306.2014.04.026

在线SPE液质联用法分析原料糖浆中2-氨基乙酰苯

1. 浙江省台州市质量技术监督检测研究院
2. 赛默飞世尔科技中国有限公司

详细信息

作者简介:
陈盛 (1983-) , 男, 硕士研究生, 研究方向:食品的检测技术研发和质量管理。;

中图分类号: O657.63;TS247
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出版历程
- 收稿日期: 2013-07-29

Determination of 2-aminoacetophenone in syrup by online SPE HPLC-MS/MS

Taizhou Institution of Quality and Technical Supervision and Inspection
Thermofisher Scientific Co., Ltd.

摘要

摘要: 建立了一种采用在线SPE对糖浆中的2-氨基乙酰苯进行了富集、浓缩与去除有机杂质干扰样品前处理方式,同时采用高效液相色谱与质谱联用仪（HPLC-MS/MS）对样品中2-氨基乙酰苯（2-AP）进行了准确定性与定量分析的方法。在线SPE柱:采用100%亲水的Acclaim PA柱（4.0mm×30mm,5.0μm）,分析柱采用ODS柱（2.1mm×150mm,3.0μm）;质谱方法,采用ESI源选择反应离子监测（SRM）模式,自动优化了S-Lens、CE等参数。结果表明:该方法的线性回归方程Y=-12123.6+33480.1X,相关系数r为0.9999,线性范围为0.3¹50ng/mL,进样体积10.0μL,检出限（以S/N=3计）为0.03ng/mL,样品加标回收率达93%以上。采用该方法对3份不同的生产工艺糖浆样品进行了分析,结果表明均小于仪器检出限。
- 2-氨基乙酰苯 /
- 在线SPE /
- 液质联用 /
- 糖浆
Abstract: An analytical method for determination of 2-aminoacetophenone in different Syrup by online SPE and HPLC MS/MS was developed which online SPE could enrich the target and remove the interference and HPLC-MS/MS could determine and quantitate of 2-aminoacetophenone. The SPE column was Acclaim PA (4.0mm×30mm) , and the analytic column was ODS (2.1mm×150mm, 3.0μm) , and the Mass Spectrometry's parameters ( S-lens, CE, etc.) were automatic optimization with SRM mode. The results showed that the calibration formula was Y=-12123.6+33480.1X, the correction coefficient was above 0.9999, and the calibration curve was linear in the range of 0.3 ¹50ng/mL, injection volume was 10.0μL and the detection limit of the method (with S/N=3) was 0.03ng/mL, the recoveries of spiked samples were more than 93%. Then 3 different samples were analyzed with this method, the contents were not detected.
- 2-ainoacetophenone /
- online SPE /
- HPLC MS/MS /
- syrup

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参考文献(7)

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