亚3微米色谱分离-串联质谱法同时筛查中药材中非法添加的30种人工色素

Simultaneous determination of thirty artificial pigments illegally added into the Chinese medicinal materials by sub-three-micron high performance liquid chromatography tandem mass spectrometry

建立了中药材中30种人工色素的高效液相色谱-串联质谱(LC-MS/MS)筛查测定方法。试验优化了前处理方法,分离条件和质谱参数。样品采用甲醇超声,提取液经亚3μm填料色谱柱Agilent Poroshell 120 EC-C18(3.0 mm×100 mm,2.7μm)分离,乙腈-水(10 mmol/L乙酸铵)为流动相梯度洗脱,流速0.30 m L/min,采用电喷雾离子源,正、负离子切换采集模式多反应选择离子监测(MRM)。30种人工色素及其中的3对同分异构体得到了理想分离和定性定量。本法简便、快速、准确可靠,已经应用于中药材中非法添加的人工色素的筛查及检测。

A method was proposed for the determination of thirty artificial pigments which were illegally added into the Chinese medicinal materials by high-performance liquid chromatograph-mass spectrometry（ LC-MS/MS）. The pretreatment methods,separation conditions and mass spectrometry parameters were optimized. The sample were extracted with methanol in ultrasonic condition,separated on a sub-three-micron Agilent Poroshell 120 EC-C18（ 3. 0 mm × 100 mm,2. 7 μm） chromatographic column with acetonitrile and water（ 10 mmol/L ammonium acetate） as mobile phases under gradient elution at a flow rate of 0. 3 m L/min. The determination was conducted by tandem mass spectrometry in positive and negative ESI mode under multiple reaction monitoring（ MRM） mode. The method exhibited ideal performance for the separation, qualification and quantification of thirty artificial pigments,especially for the three couples of isomers. The method was proved to be convenient,rapid,accurate and reliable,and it has been applied to the screening and detection of artificial pigments illegally added into the Chinese medicinal materials.