SPE-UPLC测定火锅底料中9种合成色素

Determination of 9 Synthetic Pigments in Hotpot Condiment by SPE-UPLC

建立固相萃取-超高效液相色谱法测定火锅底料中9种合成色素的分析方法。样品用乙腈-乙醇-水-氨水提取浓缩并加入甲酸,经PWA-2弱阴离子固相萃取柱富集净化,以甲醇-0.02 mol/L乙酸铵为流动相进行梯度洗脱,外标法定量,检测波长254 nm,扫描范围190~600 nm。9种色素分离效果良好,其峰面积与其质量浓度在1~50μg/mL范围内呈线性关系,相关系数R^2≥0.999,实际样品在2.0 mg/kg、5.0 mg/kg、10.0 mg/kg三个加标水平下,回收率为82%~99%,相对标准偏差(RSD)在0.1%~3%,检出限为0.05~0.25 mg/kg。

A method was developed for the determination of nine synthetic pigments in hotpot condiment by solid-phase extraction and ultra-performance liquid chromatography. The sample was extracted and concentrated with acetonitrile-ethanol-water-ammonia, and formic acid was added. The sample was enriched and purified by a PWA-2 weak anion solid phase extraction column, and methanol-0.02 mol/L ammonium acetate was used as a mobile phase for gradient elution. The detection wavelength was 254 nm and the scanning range was 190~600 nm. The separation effect of 9 kinds of pigments was good, and the peak area and its mass concentration had a linear relationship in the range of 1~50 μg/mL, and the correlation coefficient R^2≥0.999. The actual sample recovery rate was 82%~99% at the three spiked levels of 2.0 mg/kg, 5.0 mg/kg, and 10.0 mg/kg, and the relative standard deviation(RSD) was 0.1%~3%. The detection limit was 0.05~0.25 mg/kg.