液液萃取-超高效液相色谱-串联质谱法同时测定尿液中乌头碱和新乌头碱  

Simultaneous determination of aconitine and mesaconitine in urine by liquid-liquid extraction combined with ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：邓芬芳[1] 白志军[1] 谭志科[2] 王卫湛 卢祝靓子 黄淑怡 张宏峰[1] DENG Fenfang;BAI Zhijun;TAN Zhike;WANG Weizhan;LU Zhuliangzi;HUANG Shuyi;ZHANG hongfeng(Department of Physical and Chemical Analysis,Guangzhou Center for Disease Control and Prevention,Guangzhou 510440,China;Clinical Laboratory,Guangzhou Baiyun District Center for Disease Control and Prevention,Guangzhou 510445,China)

机构地区：[1]广州市疾病预防控制中心理化检验部,广州510440 [2]广州市白云区疾病预防控制中心检验科,广州510445

出　　处：《化学分析计量》2025年第1期88-92,共5页Chemical Analysis And Meterage

基　　金：广州市卫生健康科技项目(20221A011064);广州市卫生健康科技项目(20231A010043)。

摘　　要：建立液液萃取-超高效液相色谱-串联质谱法同时测定尿液中乌头碱和新乌头碱的含量。向尿液样品中加入一定量的萃取溶剂,涡旋,离心,取上层有机相,重复萃取两次,合并萃取液,氮吹至干,再复溶于乙腈中。以乙腈和含0.1%甲酸的2 mmol/L甲酸铵溶液作为流动相,梯度洗脱,采用Acquity BEH C_(18)色谱柱分离,电喷雾离子源正离子方式扫描,多反应监测模式监测,以保留时间和特征离子定性,外标法定量。乌头碱和新乌头碱的质量浓度在1.0~100.0μg/L范围内与其色谱峰面积呈良好的线性关系,相关系数均不小于0.998,方法检出限为0.01μg/L。样品加标平均回收率为99.2%~105.4%,测定结果的相对标准偏差为1.7%~4.1%(n=5)。该方法灵敏度高,准确可靠,适用于食物中毒患者尿液中乌头碱和新乌头碱的检测。A method for simultaneous determination of the content of aconitine and mesaconitine in urine by liquidliquid extraction combined with ultra high performance liquid chromatography-tandem mass spectrometry was established.A certain amount of extraction solvent was added to the urine sample.The upper organic phase was separated from urine by vortex and centrifugation.The extraction procedure was repeated twice and the two extracts were combined,evaporated with nitrogen gas to dryness.The residues were re-dissolved in acetonitrile.The mobile phase consisted of acetonitrile and 0.1%formic acid-2 mmol/L ammonium formate solution.The analytes were separated by an Acquity BEH C_(18)column with gradient elution.The compounds were identified under electrospray ionization with positive ion mode and multiple reactions monitoring mode.The analytes were qualitative analyzed by retention time and characteristic mass ion,and quantified by external standard method.The mass concentration of aconitine and mesaconitine had a good linear relationship with the chromatographic peak area in the range of 1.0-100.0μg/L,the correlation coefficients were not less than 0.998,and the detection limit of the method was 0.01μg/L.The average recoveries of sample spiked were 99.2%-105.4%,and the relative standard deviations of the determination results were 1.7%-4.1%(n=5).The method is sensitive and accurate,which is suitable for the detection of aconitine and mesaconitine in food poisoning patient's urine.

关 键 词：乌头碱 新乌头碱 液液萃取 超高效液相色谱-串联质谱 尿液 

分 类 号：O657.7[理学—分析化学]