基于液相色谱-质谱联用及^19F核磁成像技术测定一种新型氟类化合物  

Determination of a new fluorine compound by liquid chromatography-mass spectrometry and^19F nuclear magnetic imaging

作　　者：何芳菲[1] 黄平升 王婷[1] 王东亮[1] 王昱青[1] He Fang-Fei;Huang Ping-Sheng;Wang Ting;Wang Dong-Liang;Wang Yu-Qing(National Center for Nanoscience and Technology,Beijing 100090,China;Institute of Biomedical Engineering,Peking Union Medical College,Chinese Academy of Medical Sciences,Tianjin 300192,China)

机构地区：[1]国家纳米科学中心,北京100090 [2]中国医学科学院北京协和医学院生物医学工程研究所,天津300192

出　　处：《分析仪器》2020年第3期71-75,共5页Analytical Instrumentation

基　　金：中国科学院仪器设备功能开发技术创新项目(小动物磁共振小鼠多功能床的研发)。

摘　　要：(2-甲基丙烯酸乙酯)-N-(3,3,3-三氟丙基)-N-甲基甘氨酸(CBF3)是本团队新合成的一种19F核磁成像基团。本研究结合液相色谱-质谱联用方法对低浓度样品检测灵敏度高的特点,建立了CBF3液相色谱-质谱联用检测标准曲线,并进行了低、中、高3个浓度组CBF3的提取回收率和精密度等方法验证。结果表明采用液相色谱-质谱联用方法检测CBF3在浓度范围10μg/L^1000μg/L内线性关系良好,相关系数(R)大于0.995,方法定量限为10μg/L;日内精密度和日间精密度(RSD)、提取回收率均符合生物样品的分析要求。为研究CBF3在活体内的代谢情况,在小鼠给药后不同时间点,采用液相色谱-质谱联用方法进行血清CBF3浓度的定量分析,分析结果显示给药45min后血清CBF3浓度迅速下降;同时我们还采用19F核磁成像技术检测小鼠肝脏、肾脏和膀胱组织中的CBF3信号,并证明该化合物一部分可通过肝脏代谢,绝大部分经过肾脏代谢,随尿液形成蓄积在膀胱中,最终通过尿液排出体外的代谢途径。(2-(methacryloyloxy)ethyl)-N methy-N-(3,3,3-trifluoropropyl)glycine(CBF3)was a newly synthesized^19F compound by our team.In this study,the concentration of the samples was low.The standard curve of CBF3 was established,the extraction recovery and precision of CBF3 in low,medium and high concentration groups were verified.In concentration range of 10-1000μg/L the linearity rela-tionship was good,the correlation coefficient was greater than 0.995,the quantitative limit for CBF3 was determined to be 10μg/L.The intra day precision and inter day precision(RSD)and extraction recovery rates met the analysis requirements of the biological samples.In order to study the metabolism of CBF3 in-vivo,the CBF3 concentration in serum was quantitatively analyzed by liquid chromatography-mass spec-trometry at different post contrast time.The results showed that the concentration decreased rapidly after 45 minutes administration.CBF3 in mouse liver,kidney and bladder were detected by 18 F nuclear magnetic.resonance imaging.It proved that some CBF3 were metabolized by the liver,but most of them were metab-olized by the kidneys.Then CBF3 was accumulated in the bladder,and finally excreted with urine.

关 键 词：(2-甲基丙烯酸乙酯)-N-(3 3 3-三氟丙基)-N-甲基甘氨酸 液相色谱-质谱联用技术 19F核磁共振成像技术 定量分析 

分 类 号：O657.63[理学—分析化学] R965[理学—化学]