湖北农业科学 ›› 2021, Vol. 60 ›› Issue (5): 108-112.doi: 10.14088/j.cnki.issn0439-8114.2021.05.020

• 检测分析 • 上一篇    下一篇

超高效合相色谱-质谱法快速分析烟叶中游离脂肪酸

喻世涛1,2,3, 陶永峰1, 姚建武1,2,3, 魏刚1,2,3, 高颂1,2,3, 杨鑫1,2,3, 唐向兵1,2,3   

  1. 1.湖北中烟工业有限责任公司,武汉 430040;
    2.湖北新业烟草薄片开发有限公司,武汉 430056;
    3.重组烟叶应用技术研究湖北省重点实验室,武汉 430040
  • 收稿日期:2020-06-08 出版日期:2021-03-10 发布日期:2021-03-22
  • 通讯作者: 唐向兵(1965-),男,高级工程师,(电子信箱)tangxb@hbtobacco.cn。
  • 作者简介:喻世涛(1983-),男,河南信阳人,高级工程师,主要从事再造烟叶工艺质量和烟用香料提取技术研究,(电话)13707188085(电子信箱)yushitaosuccess@126.com;
  • 基金资助:
    湖北中烟工业有限责任公司资助项目(2018B032BP03)

Rapid analysis of free fatty acids in tobacco leaves by UPC2/MS

YU Shi-tao1,2,3, TAO Yong-feng1, YAO Jian-wu1,2,3, WEI Gang1,2,3, GAO Song1,2,3, YANG Xin1,2,3, TANG Xiang-bing1,2,3   

  1. 1. China Tobacco Hubei Industrial CO., Ltd., Wuhan 430040, China;
    2. Hubei Xinye Reconstituted Tobacco Development Co.,Ltd., Wuhan 430056, China;
    3. Applied Technology Research of Reconstituted Tobacco Hubei Province Key Laboratory, Wuhan 430040, China
  • Received:2020-06-08 Online:2021-03-10 Published:2021-03-22

摘要: 为快速检测分析烟叶中游离脂肪酸含量,建立了利用超高效合相色谱-质谱法(UPC2/MS)快速分析8种烟叶中棕榈酸、硬脂酸、油酸、亚油酸和亚麻酸5种脂肪酸的方法,并利用该法鉴别了32种游离脂肪酸。结果表明,采用ACQUITY UPC2色谱系统和Xevo TQS质谱仪,以HSS C18色谱柱(SB 1.8 μm, 2.1 mm×150 mm)为分析柱,以CO2和含0.1%甲酸的甲醇溶液为流动相进行梯度洗脱,5种脂肪酸在2.2~72.2 ng/mL具有较好的线性关系(r>0.999),检出限(S/N≥3)为0.06~0.13 ng/mL,定量限(S/N≥10)为0.19~0.41 ng/mL,精密度RSD为5.2%~8.0%,稳定性RSD为4.3%~7.5%,重复性试验RSD为3.0%~6.7%,不同添加水平下的平均回收率为95.8%~97.2%;8种烟叶中棕榈酸、硬脂酸、油酸、亚油酸和亚麻酸的含量在0.12~1.21 mg/g。该方法分析速度快、灵敏度高、选择性强,且样品前处理简单,无需衍生化,适用于烟叶中游离脂肪酸的测定。

关键词: 超高效合相色谱-质谱法, 烟叶, 游离脂肪酸

Abstract: In order to quickly detect and analyze the content of free fatty acids in tobacco leaves,Ultraperformance convergence chromatography mass spectrometry(UPC2/MS) was established for the rapid analysis of 5 kinds of fatty acids, palmitic acid, stearic acid, oleic acid, linoleic acid and linolenic acid, in 8 kinds of tobacco leaves, and identification of 32 kinds of free fatty acids. The results showed that HSS C18 chromatographic column (SB 1.8 μm, 2.1 mm×150 mm) was used as the analytical column, CO2 and 0.1% formic acid solution of methanol was used as the mobile phase to gradient elution by ACQUITY UPC2 chromatographic system and Xevo TQS mass spectrometer. The 5 kinds of fatty acids had a good linear relationship within the range of 2.2~72.2 ng/mL (r>0.999); the detection limit (S/N≥3) was 0.06~0.13 ng/mL; the quantitative limit (S/N≥10) was 0.19~0.41 ng/mL; the relative standard deviation (RSD) of precision was 5.2%~8.0%; the relative standard deviation (RSD) of stability was 4.3%~7.5%; the relative standard deviation (RSD) of repeatability test was 3.0%~6.7%; the average recovery rate was 95.8%~97.2% at different addition levels. The contents of palmitic acid, stearic acid, oleic acid, linoleic acid and linolenic acid in 8 tobacco leaves ranged from 0.12 mg/g to 1.21 mg/g. The method is rapid, sensitive, selective and simple in sample pretreatment without derivation. It is applicable for the determination of free fatty acids in tobacco leaves.

Key words: UPC2/MS, tobacco leaves, free fatty acids

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