高效液相色谱-飞行时间质谱测定白酒中甜蜜素

为建立高效液相色谱-四极杆-飞行时间质谱法(HPLC-Q-TOF/MS)测定白酒中甜蜜素的分析方法,试验详细优化了色谱质谱条件以及样品提取和净化条件。在该条件下,以高分辨多反应监测(MRM HR)模式扫描,外标法定量,实现了白酒中甜蜜素的精确定量分析。结果表明:甜蜜素在0~100 ng/mL范围内线性关系良好,相关系数r=0.9996。方法定量限为0.1 mg/kg,在3个添加水平下回收率为92.2%~98.9%,相对标准偏差(RSD)为2.6%~5.8%(n=6)。该方法简单、灵敏、准确性高、稳定性好,适用于白酒中甜蜜素的测定。

Determination of Sodium Cyclamate in Liquor by High-Performance Liquid Chromatography Coupled with Quadrupole-Time of Flight Mass Spectrometry

An analytical method for the determination of sodium cyclamate in liquor was established by high-performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry(HPLC-Q-TOF/MS).The HPLC-Q-TOF/MS conditions and sample extraction and purification were optimized in detail.Under these conditions,multiple reaction monitoring high-resolution(MRM HR)acquisition was performed to accurately quantify sodium cyclamate in liquor.Results showed that the linear relationship of sodium cyclamate was good in the range of 0-100 ng/mL,and the correlation coefficients(r)was 0.9996.The limit of quantitation(LOQ,S/N=10)was 0.1 mg/kg.The recoveries of sodium cyclamate at three spiked levels varied from 92.2%to 98.9%with the relative standard deviations(RSDs)ranging from 2.6%to 5.8%(n=6).The method is simple,sensitive,accurate and stable.It is suitable for the rapid determination of sodium cyclamate in liquor.