王松, 刘红斌, 崔佳丽, 周艺佳, 张光远, 梅晶, 王京昆. 藜芦胺人体血药浓度测定方法研究*[J]. 云南大学学报(自然科学版), 2018, 40(5): 979-983. doi: 10.7540/j.ynu.20180088
引用本文: 王松, 刘红斌, 崔佳丽, 周艺佳, 张光远, 梅晶, 王京昆. 藜芦胺人体血药浓度测定方法研究*[J]. 云南大学学报(自然科学版), 2018, 40(5): 979-983. doi: 10.7540/j.ynu.20180088
WANG Song, LIU Hong-bin, CUI Jia-li, ZHOU Yi-jia, ZHANG Guang-yuan, MEI Jing, WANG Jing-kun. Study on determination method of human plasma concentration of veratramine[J]. Journal of Yunnan University: Natural Sciences Edition, 2018, 40(5): 979-983. DOI: 10.7540/j.ynu.20180088
Citation: WANG Song, LIU Hong-bin, CUI Jia-li, ZHOU Yi-jia, ZHANG Guang-yuan, MEI Jing, WANG Jing-kun. Study on determination method of human plasma concentration of veratramine[J]. Journal of Yunnan University: Natural Sciences Edition, 2018, 40(5): 979-983. DOI: 10.7540/j.ynu.20180088

藜芦胺人体血药浓度测定方法研究*

Study on determination method of human plasma concentration of veratramine

  • 摘要: 研究快速、灵敏的藜芦胺人体血药浓度高效液相色谱-串联质谱(LC-MS/MS)测定方法,为藜芦胺血药浓度检测提供稳定可靠的测定方法.以非那西汀为内标,乙酸乙酯提取血浆样品,样品处理完毕后,以乙腈-10 mmol/L醋酸铵(氨水调pH至8.8)作为流动相,正离子模式下,采用多反应监测(MRM)定量,藜芦胺定量离子对m/z:410.1/295.1,非那西汀定量离子对m/z:180.2→110.0.结果表明藜芦胺在0.201~6.45ng/mL范围内线性良好,连续3批标准曲线相关系数r均大于0.99(权重1/X2),定量下限为0.201ng/mL;高、中、低3种质量浓度的日内、日间精密度(RSD)≤15.11%,准确度介于96.52%~102.42%;基质效应不影响测定.所建LC-MS/MS方法快速、灵敏、专属性强、重现性高,适用于藜芦胺人体血药浓度测定.

     

    Abstract: Objective To study the rapid and sensitive method for the determination of veratramine in human plasma by high performance liquid chromatography-tandem mass spectrometry (LC-MS/MS) and provide a stable and reliable method for the determination of veratramine blood concentration. Methods The plasma sample was extracted with ethyl acetate and phenacetin as internal standard.After the sample was processed,acetonitrile-10 mmol·L-1 ammonium acetate (pH adjusted to 8.8) was used as mobile phase.In positive ion mode,multiple reaction monitoring was used ( MRM) quantification,veratramine quantification ion pair m/z:410.1/295.1,phenacetin quantification ion pair m/z:180.2→110.0. Results Veratramine in 0.201—6.45ng/mL linear range,three consecutive batches of standard curves correlation coefficient r are greater than 0.99 (weight 1/X2),lower limit of quantitation was 0.201 ng/mL;high,medium,low three concentrations day precision (RSD%)≤15.11%,accuracy ranged between 96.52%—102.42%;the matrix does not affect the measurement effect. Conclusion The established LC-MS/MS method is rapid,sensitive,specific,and highly reproducible.It is suitable for determination of human plasma concentrations of veratramine.

     

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