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

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10~500μg/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。

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

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.