色谱

色谱 ›› 2019, Vol. 37 ›› Issue (11): 1173-1178.DOI: 10.3724/SP.J.1123.2019.05017

• 研究论文 • 上一篇    下一篇

高效液相色谱-四极杆/静电场轨道阱高分辨质谱法快速筛查保健食品中的西布曲明及其5种衍生物

洪灯, 谢文, 侯建波, 胡晓莉, 史颖珠, 李杰   

  1. 浙江省检验检疫科学技术研究院, 浙江 杭州 311215
  • 收稿日期:2019-05-17 出版日期:2019-11-08 发布日期:2020-12-11
  • 通讯作者: 洪灯.Tel:(0571)83527226,E-mail:denghong_chem@126.com.
  • 基金资助:
    浙江出入境检验检疫局项目（ZK201709）.

Rapid screening of sibutramine and five derivatives in health food by high performance liquid chromatography-quadrupole/electrostatic orbitrap high-resolution mass spectrometry

HONG Deng, XIE Wen, HOU Jianbo, HU Xiaoli, SHI Yingzhu, LI Jie   

  1. Zhejiang Academy of Science and Technology for Inspection and Quarantine, Hangzhou 311215, China
  • Received:2019-05-17 Online:2019-11-08 Published:2020-12-11
  • Supported by:
    Project of Zhejiang Entry-Exit Inspection and Quarantine Bureau (No. ZK201709).

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摘要： 建立了高效液相色谱-四极杆/静电场轨道阱高分辨质谱（HPLC-Q/Orbitrap HRMS）快速筛查保健食品中的西布曲明及其5种衍生物的方法。样品经甲醇超声提取，高速离心，Hypersil Gold色谱柱（100 mm×2.1 mm，3 μm）分离，以甲醇与0.15%（v/v）甲酸水溶液为流动相进行梯度洗脱，正离子全扫描/数据依赖二级扫描（Full MS/dd-MS2）模式下进行质谱分析，一级高分辨准分子离子峰定量。8 min内完成对样品中分析物的分离和高精度一级、二级扫描，得到准确质量数和准确碎片离子信息。实验结果表明，6种化合物的精确质量相对偏差均小于1×10-6，在0.5~20.0 μg/L范围内线性相关系数大于0.999，定量限为25 μg/kg，回收率在93.5%~103.5%，相对标准偏差在1.5%~7.7%，本方法具有前处理简单、快速、准确、高灵敏度、高选择性等特点，可用于保健食品中西布曲明及其衍生物等减肥类非法添加物的定性筛查和定量分析。

关键词: 高效液相色谱, 四极杆/静电场轨道阱高分辨质谱, 西布曲明, 衍生物, 保健食品

Abstract: A rapid screening method was developed to determine sibutramine and five derivatives in health food by high performance liquid chromatography-quadrupole/electrostatic orbitrap high-resolution mass spectrometry (HPLC-Q/Orbitrap HRMS). The sample was extracted with methanol via ultrasonic-assisted extraction coupled with high-speed centrifugation. Separation was performed on a Hypersil Gold column (100 mm×2.1 mm, 3 μm) by gradient elution with methanol/water (containing 0.15%(v/v) formic acid) as the mobile phase. The positive full mass scan/date-dependent MS2 (Full MS/dd-MS2) mode was used during MS detection, and quantification was achieved by resolution of the precursor mass. The analytes in the sample were separated, and accurate mass and MS2 fragment ions were simultaneously attained within 8 min. The results indicated that the obtained mass accuracy errors of the six analytes were less than 1×10-6. Good linearities were obtained in the range of 0.5-20.0 μg/L, and all correlation coefficients were higher than 0.999. The limits of quantification were 25 μg/kg and the recoveries were in the range of 93.5%-103.5% with relative standard deviations of 1.5%-7.7%. This simple-pretreatment, rapid, accurate, high-sensitivity, and high-selectivity method can be used in the rapid screening and quantitative analysis of sibutramine and its derivatives in health food.

Key words: high performance liquid chromatography (HPLC), quadrupole/electrostatic orbitrap high-resolution mass spectrometry (Q/Orbitrap HRMS), sibutramine, derivatives, health food

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