液质联用色谱法同时测定微透析样品中尼古丁与氘代尼古丁的含量  

Development of LC-MS/MS Method for Simultaneous Determination of Nicotine and DL-Nicotine in Microdialysis Samples

作　　者：凌家俊[1] 陈亮[1] 徐晖[2] 

机构地区：[1]广州中医药大学中药学院,广东广州510006 [2]广州中医药大学中药资源研究与工程中心,广东广州510006

出　　处：《现代中药研究与实践》2010年第6期71-74,共4页Research and Practice on Chinese Medicines

基　　金：国家自然科学基金(项目编号:30772791)

摘　　要：目的建立液质联用法同时测定微透析样品中尼古丁与稳定同位素氘取代尼古丁的含量。方法色谱采用Hypersil Gold C18柱(150mm×2.1mm,3μm);流动相:甲醇-2mmol·L-1乙酸铵(70:30);流速:0.21mL·min-1;质谱条件:大气压电喷雾离子源(ESI),正离子模式,选择离子反应监测;定量离子对分别是:尼古丁m/z163/130,氘代尼古丁m/z166/130。结果尼古丁在0.140-53.085ng、氘代尼古丁在0.148-50.19ng范围内线性关系良好,定量下限分别为尼古丁0.140ng(S/N>10),氘代尼古丁0.148ng(S/N>10);日内、日间精密度均小于15%。结论本方法灵敏度高、专属性好,操作简便、快速,适于微透析样品中尼古丁与氘取代尼古丁含量的测定。Objective To develop a LC-MS/MS method for simultaneous determination of Nicotine and DL-Nicotine in microdialysis samples.Methods An HPLC method was performed on a Hypersil Gold C18 column（150 mm×2.1 mm,3 μm） with methanol-2 mmol·L^-1 ammonium acetate（70：30） as mobile phase.The · ow rate was 0.21 mL·min^-1.Mass spectra were measured by a triple quadrupole mass spectrometer equipped with an electrospray ionization（ESI） source,in positive ion model.In selected reaction monitoring（SRM） mode,the transitions of m/z 163 to 130,m/z 166 to 130 was used to quantify nicotine and DL-nicotine,respectively.Results The calibration curve was in good linearity over the range of 0.140-53.085 ng·mL^-1（Nicotine）,and 0.148-50.19 ng·mL^-1（DL-Nicotine）.The lower limit of quantification is 0.140 ng·mL^-1（Nicotine,S/N〉10）,and 0.148 ng·mL^-1（DL-Nicotine,S/N〉10）.Both the intra and inter-day precisions（RSD） were less than 15%.Conclusion The proposed method is speedy,sensitive and accurate.It is suitable for determination of Nicotine and DL-Nicotine in microdialysis samples.

关 键 词：尼古丁 氘取代尼古丁 液质联用 

分 类 号：R927.1[医药卫生—药学]