食品科学 ›› 2017, Vol. 38 ›› Issue (24): 196-201.doi: 10.7506/spkx1002-6630-201724031

• 安全检测 • 上一篇    下一篇

超高效液相色谱-四极杆/静电场轨道离子阱质谱测定植物提取物中的7 种合成色素

朱振宝,张亚莉,贾玮,孔祥虹,何强   

  1. (1.陕西科技大学食品与生物工程学院,陕西?西安 710021;2.陕西省出入境检验检疫分析中心食品实验室,陕西?西安 710068)
  • 出版日期:2017-12-25 发布日期:2017-12-07
  • 基金资助:
    国家自然科学基金面上项目(31671888);陕西省自然科学基金面上项目(2015JM3085)

Determination of 7 Artificial Dyes in Plant Extracts by Ultra-Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbit Trap High-Resolution Mass Spectrometry

ZHU Zhenbao, ZHANG Yali, JIA Wei, KONG Xianghong, HE Qiang   

  1. (1. School of Food Science and Bioengineering, Shaanxi University of Science and Technology, Xi’an 710021, China; 2. Food Inspection Center of Shaanxi Entry-Exit Inspection and Quarantine Bureau, Xi’an 710068, China)
  • Online:2017-12-25 Published:2017-12-07

摘要: 基于高分辨质谱,建立植物提取物中7?种合成色素的快速检测方法。样品经超纯水提取,采用聚酰胺固相萃取小柱净化,以C18色谱柱为分析柱,乙腈和5?mmol/L乙酸铵溶液作为流动相,经超高效液相色谱进行梯度洗脱分离,利用四极杆静电场轨道离子阱质谱测定。结果表明:在10~500?μg/mL范围内,7?种限用及禁用合成色素线性关系良好,相关系数(r2)均大于0.99。通过加标验证实验,在0.05、0.1、0.5?mg/kg?3?个加标水平下,该方法的检出限可达到0.001?2~0.052?mg/kg,加样回收率为60.8%~91.8%,相对标准偏差为2.1%~6.5%。通过实际样品检测,结果表明本方法样品处理过程简单,分析时间短,准确可靠,灵敏度高,适用于植物提取物中合成色素的快速筛查及确证。

关键词: 植物提取物, 合成色素, 超高效液相色谱-四极杆/静电场轨道离子阱质谱, 高分辨质谱

Abstract: A rapid method was presented for the determination of 7 artificial dyes in plant extracts by ultra-performance liquid chromatography-electrospray ionization quadrupole orbitrap high-resolution mass spectrometry (UPLC-Q-Orbitrap-MS). Samples were extracted with water, and the extract was cleaned up on a polyamide solid phase extraction (SPE) column and separated by UPLC on a C18 column using a mobile phase consisting of 5 mmol/L ammonium acetate-acetonitrile with gradient elution. Data were collected by ESI Q-Orbitrap MS. The results showed that good linearity was observed in the concentration range from 10 to 500 μg/mL for all 7 artificial dyes, with correlation coefficients (r2) greater than 0.99. The limits of detection (LODs) ranged from 0.001 2 to 0.052 mg/kg. The average recoveries were in the range from 60.8% to 91.8% at 3 spiked levels with relative standards deviation (RSDs) between 2.1% and 6.5%. This method proved to be simple, time saving, accurate, reliable and sensitive and thus can be used for the fast screening and confirmation of artificial dyes in plant extracts.

Key words: plant extracts, artificial dyes, ultra-performance liquid chromatography-quadrupole/electrostatic field orbit trap mass spectrometry, high-resolution mass spectrometry

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