液相色谱-串联质谱法检测芝麻糊样品中东莨菪碱、消旋山莨菪碱和阿托品  

Determination of scopolamine,racanisodamine and atropine in sesame paste by liquid chromatography-tandem mass spectrometry

作　　者：邓淑铃 朱峰 张昊 王溪 刘华良 DENG Shuling;ZHU Feng;ZHANG Hao;WANG Xi;LIU Hualiang(School of Public Health,Nanjing Medical University,Nanjing 211166,China;Jiangsu Provincial Center for Disease Control and Prevention,Nanjing 210009,China)

机构地区：[1]南京医科大学公共卫生学院,南京211166 [2]江苏省疾病预防与控制中心理化检验所,南京210009

出　　处：《化学分析计量》2025年第2期18-24,共7页Chemical Analysis And Meterage

基　　金：江苏省重点研发计划(社会发展)项目(BE2023720)。

摘　　要：建立基于QuEChERS原则快速提取净化芝麻糊样品,液相色谱-串联质谱(LC-MS/MS)法同时检测东莨菪碱、消旋山莨菪碱和阿托品的方法。以含20%(体积分数)甲酸的乙腈溶液提取芝麻糊样品,经EMR-Lipid以及Mg_(2)SO_(4)、PSA和C_(18)净化,选取ACQUITYUPLCBEHC_(18)(100 mm×2.1 mm,1.7μm)色谱柱,以甲酸(0.1%,体积分数)水-甲醇溶液为流动相梯度洗脱,电喷雾离子源正离子多反应监测模式采集,基质匹配校准曲线法定量。在质量浓度0.1~10 ng/m L内,东莨菪碱、消旋山莨菪碱和阿托品与对应色谱峰面积呈现良好的线性关系,相关系数均大于0.999。检出限为0.02~0.03μg/kg,定量限为0.08~0.10μg/kg。3种生物碱在低、中、高三个不同加标浓度水平的平均回收率为79.8%~110%,测量值的相对标准偏差为2.1%~7.0%(n=6)。该方法耗时较短,定性可靠、定量准确,适用于各类食品制品曼陀罗有毒植物中毒的应急检测。A rapid extraction and purification method for sesame paste samples based on QuEChERS principle was established,and liquid chromatography-tandem mass spectrometry(LC-MS/MS)was used to simultaneously detect scopolamine,anisodamine and atropine.The sesame paste samples were extracted with 20%(volume fraction)formic acid acetonitrile solution and purified by EMR-Lipid,Mg_(2)SO_(4),PSA and C_(18).ACQUITY UPLC BEH C18(100 mm×2.1 mm,1.7μm)was selected as the chromatographic column,and formic acid(0.1%,volume fraction)water-methanol solution was used as the mobile phase for gradient elution.The electrospray ion source was collected in the positive ion multi-reaction monitoring mode,and the matrix matching calibration curve method was used for quantification.In the mass concentration range of 0.1-10 ng/mL,scopolamine,anisodamine and atropine showed good linear relationships with the corresponding chromatographic peak areas,and the correlation coefficients were all greater than 0.999.The limit of detection were 0.02-0.03μg/kg,the limit of quantification were 0.08-0.10μg/kg.The average recoveries of the three alkaloids at the low,medium and high spiked concentration levels were 79.8%-110%,and the relative standard deviations were 2.1%-7.0%(n=6).The method is less time-consuming,qualitatively reliable,quantitatively accurate,which is suitable for emergency detection of toxic plant poisoning of various food products.

关 键 词：液相色谱-串联质谱法 芝麻糊 东莨菪碱 消旋山莨菪碱 阿托品 

分 类 号：O657.7[理学—分析化学]