UPLC-MS/MS法测定配制酒中黄芪甲苷的含量

Determination of Astragaloside Ⅳ in Liqueur by UPLC-MS/MS

建立了配制酒中黄芪甲苷的超高效液相色谱-串联质谱(UPLC-MS/MS)测定方法。经水浴挥干后的配制酒样品用含4%浓氨试液的80%甲醇水溶液提取净化,以ACQUITY UPLC HSS T3 C_(18)色谱柱(1.8μm,100 mm×2.1 mm)分离,流动相为乙腈-0.1%甲酸水(梯度洗脱),电喷雾正离子模式(ESI+)检测,多反应离子检测模式(MRM)定量分析。结果显示:该方法在1.0~20 mg/L范围内线性关系良好,相关系数R^(2)为0.9992,线性方程为y=1017.4x+45.04,方法检出限为0.10 mg/kg;仪器精密度良好,峰面积RSD为3.76%(n=6);方法重复性良好,配制酒中黄芪甲苷含量RSD为2.1%(n=6);配制酒中3个加标水平下的平均回收率范围83.5%~104.1%(n=6);相对标准偏差为3.7%~7.2%。该方法灵敏度高、分析时间短、稳定性好,是测定配制酒中黄芪甲苷含量的有效方法。

In this study we established a UPLC-MS/MS method for the determination of astragalosideⅣcontent in liqueur.The experimental samples were extracted and purified with 80%methanol aqueous solution containing 4%ammonia.Then the samples were separated on an ACQUITY UPLC HSS T3 C_(18) column(1.8μm,100 mm×2.1 mm)by gradient elution with acetonitrile-0.1%formic acid aqueous solution.Electrospray ionization in the positive ion mode(ESI+)was used for detection.Quantitative analysis was done with multiple reactions monitoring(MRM).The results showed that the method had good linear relationship in the range of1.0 mg/L to 20 mg/L,and the correlation coefficient was 0.9992(y=1017.4 x+45.04).The limit of detection was 0.10 mg/kg.The precision of the instrument was good.The RSD value of the peak area was 3.76%(n=6),and the method had good repeatability.The RSD value of astragalosideⅣcontent in liqueur was 2.1%(n=6).The average recoveries of the three spiking levels ranged from83.5%to 104.1%(n=6),and the RSD values ranged from 3.7%to 7.2%.The method had high sensitivity,short analysis time and good stability,and could be used to determine the content of astragalosideⅣin liqueur.