高效液相色谱-串联质谱法测定高粱中蜀黍苷的含量

建立了高粱中蜀黍苷的高效液相色谱-串联质谱(HPLC-MS/MS)检测方法。样品经甲醇-水(95∶5,v/v)提取,C18色谱柱分离,HPLC-MS/MS多反应离子监测(MRM)方式检测,并采用外标法定量。结果表明,蜀黍苷在浓度10.1~202μg/L范围内时与其峰面积呈良好线性关系,相关系数不低于0.999,检出限为0.178μg/L,定量限为0.593μg/L,低、中、高3个不同水平的加标回收率分别为96.1%、97.9%、90.7%,重复性好,精密度高。所建立的方法具有前处理简单、准确性好、灵敏度高的特点,可用于高粱中蜀黍苷的定量分析。

Determination of Dhurrin Content in Sorghum by HPLC-MS/MS

The determination method of dhurrin content in sorghum by HPLC-MS/MS had been developed.The sample was extracted with methanol-water(95∶5,v/v),separated by C18 column,detected by HPLC-MS/MS multi-reaction ion monitoring(MRM),and quantified by external standard method.The results showed that,the concentration of dhurrin in the range of 10.1μg/L to 202μg/L showed a good linear relationship with the peak area,the correlation coefficient was not lower than 0.999,the detection limit was 0.178μg/L,the limit of quantification was 0.593μg/L,and the recoveries of low,medium and high levels were 96.1%,97.9%and 90.7%respectively with good repeatability and high precision.The method had the characteristics of simple pretreatment,high accuracy and high sensitivity,and could be used for quantitative analysis of dhurrin in sorghum.