首页> 外文期刊>Journal of separation science. >Simultaneous analysis of gemfibrozil, morphine, and its two active metabolites in different mouse brain structures using solid-phase extraction with ultra-high performance liquid chromatography and tandem mass spectrometry with a deuterated internal standard
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Simultaneous analysis of gemfibrozil, morphine, and its two active metabolites in different mouse brain structures using solid-phase extraction with ultra-high performance liquid chromatography and tandem mass spectrometry with a deuterated internal standard

机译:使用超高效液相色谱固相萃取和氘代内标串联质谱法同时分析不同小鼠大脑结构中的吉非贝齐,吗啡及其两种活性代谢物

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A rapid and sensitive bioassay was established and validated to simultaneously determine gemfibrozil, morphine, morphine-3 beta-glucuronide, and morphine-6 beta-glucuronide in mouse cerebrum, epencephalon, and hippocampus based on ultra-high performance liquid chromatography and tandem mass spectrometry. The deuterated internal standard, M6G-d3, was mixed with the prepared samples at 10 ng/mL as the final concentration. The samples were transferred into the C-18 solid-phase extraction columns with gradient elution for solid-phase extraction. The mobile phase consisted of methanol and 0.05% formic acid (pH 3.2). Multiple reaction monitoring has been applied to analyze gemfibrozil (m/z 249.0 -> 121.0) in anion mode, and M6G-d3 (m/z 465.1 -> 289.1), morphine (m/z 286.0 -> 200.9), and M3G and M6G (m/z 462.1 -> 286.1) in the positive ion mode. The method has a linear calibration range from 0.05 to 10 ng for gemfibrozil, morphine, and M3G and M6G with correlation coefficients >0.993. The lower limit of quantitation for all four analytes was 0.05 ng/mL, relative standard deviation of intra-and interday precision was less than 10.5%, and the relative error of accuracy was from -8.2 to 8.3% at low, medium, and high concentrations for all the analytes. In conclusion, gemfibrozil can influence the morphine antinociception after coronary heart disease induced chronic angina by the change in one of morphine metabolites', M3G, distribution in mouse brain.
机译:建立了快速灵敏的生物测定方法,并通过超高效液相色谱和串联质谱法同时测定了小鼠大脑,脑中脑和海马体中的吉非贝齐,吗啡,吗啡3β-葡萄糖醛酸和吗啡6β-葡萄糖醛酸含量,并进行了验证。 。将氘化内标M6G-d3与制备的样品以最终浓度10 ng / mL混合。样品通过梯度洗脱转移到C-18固相萃取柱中进行固相萃取。流动相由甲醇和0.05%甲酸(pH 3.2)组成。多反应监测已应用于阴离子模式下的吉非贝齐(m / z 249.0-> 121.0),M6G-d3(m / z 465.1-> 289.1),吗啡(m / z 286.0-> 200.9),M3G和M6G(m / z 462.1-> 286.1)在阳离子模式下。该方法对吉非贝齐,吗啡,M3G和M6G的线性校准范围为0.05至10 ng,相关系数> 0.993。四种分析物的定量下限均为0.05 ng / mL,日内和日间精密度的相对标准偏差小于10.5%,低,中和高浓度时的相对准确度误差为-8.2至8.3%所有分析物的浓度。总之,吉非贝齐可通过改变吗啡代谢产物之一M3G在小鼠脑中的分布来影响冠心病诱发慢性心绞痛后的吗啡镇痛作用。

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