微波辅助萃取-液质联用法快速检测食品种九种维生素

Rapid Detection of Nine Vitamins in Food by Microwave Assisted Extraction-LC-MS Method

本研究建立了一种使用微波辅助萃取-液质联用法快速检测食品中九种维生素含量的方法:样品中目标物经pH为4.5甲醇水溶液微波加速萃取,采用Waters ACQUITY UPLC■HSS T3(2.1 mm×100 mm×1.8μm)色谱柱进行分离,流动相为20 mM乙酸铵-0.1%甲酸水溶液-0.1%甲酸甲醇溶液,梯度洗脱;流速0.3 mL/min;柱温40℃;多反应监测模式(multiple reaction monitoring,MRM)定量分析。结果表明,在最优条件下,该方法中所有药物成分均在10~200 ng/mL范围内线性良好,相关系数R^(2)均大于0.999,方法检出限均低于1.0 ng/mL,定量限均低于3.0 ng/mL,回收率均在80%~110%之间,连续六次平行实验结果之间的相对标准偏差均<10%。该方法灵敏度高,选择性好,结果准确可靠,可同时快速检测各种食品中9种维生素的含量。

This study established a method to rapidly detect the content of nine vitamins in food using microwave-assisted extraction-LC-MS:the target substances in the sample were extracted by microwave through the methanol aqueous solution with a pH of 4.5 in an accelerated manner,and were separated with the use of Waters ACQUITY UPLC■ HSS T3(2.1 mm×100 mm×1.8μm)chromatographic column.Then the ammonium acetate-0.1%formic acid aqueous solution-0.1% formic acid methanol solution with a mobile phase of 20 mM was used for gradient elution,with a flow rate of 0.3 mL/min and a column temperature of 40℃.In the end,the multiple reaction monitoring(MRM)quantitative analysis was conducted.The results showed that under optimal conditions,all pharmaceutical ingredients in this method had good linearity in the range of 10 to 200 ng/mL,the correlation coefficients R^(2) were all higher than 0.999,the detection limits of the method were all lower than 1.0 ng/mL,the quantification limits were all lower than 3.0 ng/mL,the recovery rates were all between 80% and 110%,and the relative standard deviations between the results of six consecutive parallel experiments were all<10%.This method has high sensitivity,good selectivity,accurate and reliable results,and is able to quickly detect the contents of 9 vitamins in various foods at the same time.