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超高效液相色谱串联质谱测定儿童血液样本中高三尖杉酯碱含量OACSTPCD

Determination of Harringtonine in Blood Samples of Children by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

中文摘要英文摘要

目的:建立并验证超高效液相色谱串联质谱(UPLC-MS/MS)测定儿童血液样本中高三尖杉酯碱含量的方法.方法:以Waters Xevo TQD为检测设备,Waters BEH C18(100 mm ×2.1 mm,1.7 μm)为色谱柱,采用甲醇为有机相,含0.1%甲酸的超纯水为无机相,进行梯度洗脱,质谱检测采用正离子,多重反应监控(MRM)模式,待测物高三尖杉酯碱(HHT)离子通道m/z 546.3→298.2,内标物三尖杉酯碱(HT)离子通道m/z 532.2→298.3,锥孔电压50 V,碰撞能量28 V.结果:本方法样本前处理简单,分析速度快,结果具有较高的选择性和灵敏度,线性区间0.5~120.0ng,线性方程Y=0.047 011 3X+0.007 035 8(r=0.999 1),定量下限0.5 ng,日内精密度RSD<8.16%,日间精密度RSD<6.38%,准确度94.00%~103.95%.结论:本方法选择性好、灵敏度高,可应用于儿童体内HHT的药动学研究和血药浓度监测等相关工作.

Objective:To establish and verify ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method for content determination of homoharringtonine in blood sample of children.Methods:Waters Xevo TQD was used as detection equipment,with Waters BEH C18(100 mm ×2.1 mm,1.7 μm)as separation column.Methanol as organic phase and ultra-pure water containing 0.1%formic acid as inorganic phase were used for gradient elution.Mass detection type was positive mode,with multiple reaction monitoring(MRM).The detection ion pair of harringtonine(HHT)was 546.3→298.2,the detection ion pair of internal standard harringtonine(HT)was 532.2→298.3,the cone energy was 50 V,and the collision energy was 28 V.Results:This method was characterized by simple sample pretreatment,fast analysis speed,and high selectivity and sensitivity,with a linear interval of 0.5 to 120.0 ng,a linear equation of Y=0.047,011,3X+0.007,035,8(r=0.999,1),a lower limit of quantification of 0.5 ng,an intra-day precision of RSD<8.16%,an inter-day precision of RSD<6.38%,and an accuracy of 94.00% to 103.95%.Conclusion:This method is selective and sensitive,and can be applied to the pharmacokinetic study of HHT in children and the monitoring of blood drug concentration and other related work.

袁树伟;杜小换;张先明;花盛浩;胡绍燕;朱增燕

苏州大学附属儿童医院,江苏苏州 215123

药学

超高效液相色谱串联质谱高三尖杉酯碱药代动力学

ultra-high performance liquid chromatography-tandem mass spectrometryhomoharringtoninepharmacokinetics

《儿科药学杂志》 2024 (003)

16-19 / 4

2023年度苏州市科技发展计划指导性项目,编号SKJD2023192.

10.13407/j.cnki.jpp.1672-108X.2024.03.004

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