摘要
目的建立液相色谱-多级多反应监测模式(liquid chromatography-multiple-reaction monitoring cubed,LC-MRM^(3))同时测定中草药和药酒中3种强心作用的生物碱(欧夹竹桃苷、欧夹竹桃苷乙和去甲乌药碱)。方法样品用80%甲醇提取后经30%乙腈稀释后直接进样,在Phenomenex Kinetex C_(18)色谱柱(100×2.1 mm,2.6μm)上进行梯度洗脱,分离后采用LC-MRM^(3)模式检测。结果3种生物碱在相应的浓度范围内呈良好的线性关系(r>0.999),药酒样品检出限为0.019~0.071μg/L,草药样品检出限为0.006~0.022μg/kg,加标回收率为90.31%~97.92%,相对标准偏差为1.14%~2.73%(n=6)。与传统的液相色谱-多反应监测模式(liquid chromatography-multiple-reaction monitoring,LC-MRM)方法相比,LC-MRM^(3)方法的检测灵敏度提升约一个数量级,并且允许简单的样品制备,而不会有基质效应的影响。定性结果通过多级串联质谱(multi-stage mass spectrometry,MS3)扫描得到进一步确认。LC-MRM^(3)的定量结果与LC-MRM的结果基本一致。结论该方法简便、快速、可靠,可用于同时检测中草药和药酒中3种强心作用的生物碱。
Objective To establish a liquid chromatography-multiple-reaction monitoring cubed(LC-MRM^(3))methods for the simultaneous determination of three cardiotonic alkaloids in Chinese herbal medicine and medicinal liquor(Oleandrin,Adynerin and Higenamine).Methods The samples were extracted with 80%methanol,diluted with 30%acetonitrile,and then directly injected.Gradient elution was performed on a Phenomenex Kinetex C_(18) chromatographic column(100×2.1 mm,2.6μm),and after separation,detected using the LC-MRM^(3) mode.Results The three alkaloids showed good linear relationships within their respective concentration ranges(r>0.999).The detection limits in medicinal liquor samples ranged from 0.019 to 0.071μg/L,for Chinese herbal medicine samples,the detection limits ranged from 0.006 to 0.022μg/kg.The spike recovery rate was 90.31%-97.92%,with a relative standard deviation of 1.14%-2.73%(n=6).Compared to the traditional method liquid chromatography-multiplereaction monitoring(LC-MRM),the LC-MRM^(3) method enhanced the detection sensitivity by an order of magnitude and allowed for simple sample preparation without the impact of matrix effects.Qualitative results were further confirmed through multi-stage mass spectrometry(MS3)scanning.The quantitative results of LC-MRM^(3) were essentially consistent with those of LC-MRM.Conclusion This method is simple,fast,and accurate,and can be used for the simultaneous detection of three cardiotonic alkaloids in Chinese herbal medicine and medicinal liquor.
作者
覃昆飞
黄丽珍
何建忠
QIN Kunfei;HUANG Lizhen;HE Jianzhong(Department of Physical and Chemical Laboratory,Guigang Center for Disease Control and Prevention,Guigang,Guangxi 537100,China)
出处
《职业与健康》
CAS
2024年第17期2337-2345,共9页
Occupation and Health
基金
广西壮族自治区卫健委自筹经费科研项目(Z20211584)。
