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UPLC-MS/MS法测定配制酒中黄芪甲苷的含量 被引量:2

Determination of Astragaloside Ⅳ in Liqueur by UPLC-MS/MS
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摘要 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.
作者 兰余 胡中海 王丹 吴小娟 吉喆 吴卫宇 刘小刚 罗爽 袁强 马康 张琴 曹晓念 LAN Yu;HU Zhonghai;WANG Dan;WU Xiaojuan;JI Zhe;WU Weiyu;LIU Xiaogang;LUO Shuang;YUAN Qiang;MA Kang;ZHANG Qin;CAO Xiaonian(Luzhou Laojiao Co.Ltd.,Luzhou,Sichuan 646000;Sichuan Quality Inspection Co.Ltd.,Luzhou,Sichuan 646000;Luzhou Laojiao Health Liquor Co.Ltd.,Luzhou,Sichuan 646000,China)
出处 《酿酒科技》 2021年第7期130-134,142,共6页 Liquor-Making Science & Technology
关键词 UPLC-MS/MS法 黄芪甲苷 配制酒 UPLC-MS/MS astragalosideⅣ liqueur
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