摘要
Liquid chromatography coupled with the triple quadrupole mass spectrometry(LC-QQQ MS)technique is the most commonly used technique for quantitative analysis.It is widely used in pharmacology,targeted metabolomics,Chinese medicine quality control,and other research fields.The technique monitors only characteristic precursors and product ions through multiple reaction monitoring(MRM)mode and can detect targeted molecules in complex matrix with high specificity and sensitivity.In the present study,a diarylamide derivative diuretic was used as an example to introduce the method establishment and parameter optimization of this liquid chromatography-mass spectrometry technique.Diuretic and its internal standard could be completely separated within a 5-min gradient,and the quantitative linear range was 1–1000 ng/mL with R2=0.9996 in practical samples.This study showed that the key to the method development for LC-QQQ MS was the selection of the LC mobile phase,the elution gradient,the declustering potential,and the collision energy of compounds in MS.
液相色谱-三重四极杆串联质谱(LC-QQQ MS)技术是最常用的液质定量分析技术,广泛应用于药理学、靶向代谢组学、中药质量控制等研究领域。该技术利用多反应监测(MRM)模式,只对特定的母离子和子离子通道进行扫描监测,能够在复杂基体中高特异性、高灵敏度检测到靶标分子。本研究以一种二芳基酰胺类利尿药为实验对象,介绍液相色谱和质谱部分的方法建立和参数优化。利尿药和内标可以在5分钟梯度内完全分离,定量线性范围为1–1000 ng/mL(R^(2)=0.9996)。优化结果表明,液相色谱的流动相选择、洗脱梯度设置和质谱中化合物的去簇电压、碰撞能的设定是液相色谱-三重四极杆串联质谱方法学建立的关键。
基金
National Natural Science Foundation of China(Grant No.22004004 and 81620108029).
