摘要
用液相色谱-电喷雾离子阱质谱(LC/ESI-ITMS)建立了一种灵敏、快速可靠的分析烟草游离茄尼醇的方法。烟草样品用85%甲醇-15%异丙醇(V/V)超声萃取30 min,在分析前无需进行其他前处理。在1.8μm快速分离C18色谱短柱上用85%甲醇-15%异丙醇作为流动相等梯度洗脱实现了茄尼醇的快速分离。在电喷雾正电离模式下,用不带碰撞能量的二级质谱全扫描选择监测离子[M+Na]+(m/z 653.8)进行定量。方法的最低检测限(LOD)为5 ng/mL,日内精密度和日间精密度分别为3.7%和5.0%。两种添加量的回收率分别为96%和102%。方法成功的应用于检测多种烟草样品。
A rapid,sensitive and reliable liquid chromatography / electrospray ionization-ion trap mass spectrometry（LC/ESI-ITMS） method was developed for the determination of free solanesol in tobacco.Solanesol was efficiently extracted by ultrasonic extraction from tobacco with methanol？isopropanol（85：15,V/V） for 30 min and no further workup procedure was needed before analyzed.Solanesol was separated by using a short 1.8 ？m rapid separation C18 column with methanol？isopropanol（85：15,V/V） as the mobile phase in the isocratic gradient to achieve a fast chromatographic analysis.In the positive ESI mode,the sodium adduct ion（＋,m/z 653.8） selected for quantitation was sensitively detected in the two-stage mass（MS2） full scan mode without employing collision energy.The limit of detection（LOD） was 5 ng/mL.The intra-day and the inter-day precision were 3.7% and 5.0%,respectively.The recoveries were 96% and 102% for two different spiked levels.The established method has been successfully applied to the determination of solanesol in various tobacco samples.
出处
《现代食品科技》
EI
CAS
2011年第5期598-600,共3页
Modern Food Science and Technology
关键词
液相色谱
电喷雾离子化
离子阱质谱
茄尼醇
烟草
liquid chromatography
electrospray ionization
Ion trap mass spectrometry
solanesol
tobacco
