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目的建立同时测定枸杞中15种染料和色素的超快速液相色谱-串联质谱分析方法(LC-MS/MS)。方法样品用水浸泡后,用自制的功能化氨基磁性高分子复合微粒(EDA-MPs)进行分散固相萃取。以乙腈和5 mmol/L乙酸铵水溶液为流动相,采用梯度洗脱方式在Shim-pack XR-ODS II色谱柱(75 mm×2.0 mm,2.2μm)上进行分离,以电喷雾负离子模式进行质谱检测。结果 15种待测化合物在检测范围内均具有良好的线性关系(r>0.999),方法的定量限为0.5~10.0μg/kg,检出限为0.2~3.0μg/kg,样品的回收率为90.3%~108.7%,RSDs为2.07%~6.20%。结论LC-MS/MS法分析速度快、重现性好、灵敏度高,可用于枸杞中15种染料和合成色素的检测。
Objective To establish an LC-MS / MS method for the simultaneous determination of 15 dyes and pigments in Lycium barbarum. Methods The samples were immersed in water and dispersed solid-phase extraction was carried out by self-made functionalized magnetic polymer magnetic nanoparticles (EDA-MPs). The separation was performed on a Shim-pack XR-ODS II column (75 mm × 2.0 mm, 2.2 μm) by gradient elution using acetonitrile and 5 mmol / L ammonium acetate as the mobile phase. The mass spectra were performed by electrospray negative ion mode Detection. Results The 15 compounds tested had a good linear relationship (r> 0.999) in the detection range. The limit of quantification was 0.5-10.0μg / kg and the detection limit was 0.2-3.0μg / kg. The recovery rate of the sample was 90.3% ~ 108.7%, RSDs 2.07% ~ 6.20%. Conclusion LC-MS / MS method has the advantages of fast analysis, good reproducibility, high sensitivity and can be used for the detection of 15 kinds of dyes and synthetic pigments in Chinese wolfberry.