超高效液相色谱-串联质谱法快速测定香精中香豆素的含量
UHPLC-MS/MS Determination of Coumarin in Essence
-
摘要: 香精经乙醇提取,采用超高效液相色谱-串联质谱快速测定了香精中香豆素的含量.以ACQUITYTM BEH C18分离柱,以乙腈和乙酸为流动相梯度洗脱,采用多反应监测正离子模式检测,定量离子对为m/z 147.2,65.0,定性离子对为m/z 147.2,91.0.线性范围为20~8 000 μg·L-1,检出限(3S/N)为10 μg·L-1.加标回收率在96.6%~101.0%之间,相对标准偏差(n=5)为3.9%~5.7%.Abstract: The sample of essence was extracted with ethanol,and the solution obtained was determined rapidly by UPLC. The ACQUITYTM BEH C18 column was used as stationary phase;and a mixture of acetonitrile and acetic acid was used as mobile phase;positive electrospray ionization as well as multiple reaction monitoring mode was used in the detection. Ion pair used for qualitative analysis was: m/z 147.2,65.0,ion pair use for quantitative analysis was m/z 147.2,91.0. Linearity range was found between 20-8 000 μg·L-1,and the detection limit (3S/N) found was 10 μg·L-1. Values of recovery found by addition of standard coumarin were found in the range of 96.6%-101.0%,and values of RSD (n=5) was in the range of 3.9%-5.7%.