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Analysis of Flavonoids in Dalbergia odorifera by Ultra-Performance Liquid Chromatography with Tandem Mass Spectrometry

机译:高效液相色谱-串联质谱法分析黄檀中的类黄酮

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摘要

, a traditional Chinese medicine, has been used to treat cardio- and cerebrovascular diseases in China for thousands of years. Flavonoids are major active compounds in . In this paper, a rapid and sensitive ultra-high performance liquid chromatography-triple quadrupole mass spectrometry method was developed and validated for simultaneous determination of 17 flavonoids in . Quantification was performed by multiple reaction monitoring using electrospray ionization in negative ion mode. Under the optimum conditions, calibration curves for the 17 analytes displayed good linearity ( > 0.9980). The intra- and inter-day precisions (relative standard deviations) were lower than 5.0%. The limit of quantitation ranged from 0.256 to 18.840 ng/mL. The mean recovery range at three spiked concentrations was 94.18–101.97%. The validated approach was successfully applied to 18 samples of . Large variation was observed for the contents of the 17 analytes. Sativanone and 3′- -methylviolanone were the dominant compounds. The fragmentation behaviors of six flavonoids were investigated using UPLC with quadrupole time-of-flight tandem mass spectrometry. In negative ion electrospray ionization mass spectrometry, all the flavonoids yielded prominent [M − H] ions. Fragments for losses of CH , CO, and CO were observed in the mass spectra. Formononetin, liquiritigenin, isoliquiritigenin, sativanone, and alpinetin underwent retro-Diels–Alder fragmentations. The proposed method will be helpful for quality control of .
机译:作为一种传统中药,在中国已经用于治疗心脑血管疾病已有数千年的历史了。黄酮类是黄酮类化合物中的主要活性化合物。本文建立了一种快速灵敏的超高效液相色谱-三重四极杆质谱法,并验证了该方法可同时测定中的17种黄酮。使用负离子模式下的电喷雾电离,通过多反应监测进行定量。在最佳条件下,这17种分析物的校准曲线显示出良好的线性(> 0.9980)。日内和日间精度(相对标准偏差)均低于5.0%。定量限为0.256至18.840 ng / mL。在三个加标浓度下的平均回收率范围为94.18-101.97%。经过验证的方法已成功应用于18个样品。观察到17种分析物的含量差异很大。 Sativanone和3'--甲基维拉酮是主要化合物。使用UPLC和四极杆飞行时间串联质谱法研究了六个类黄酮的碎裂行为。在负离子电喷雾质谱中,所有类黄酮均产生显着的[MH]离子。在质谱图中观察到了CH,CO和CO损失的碎片。 Formononetin,liquiritigenin,isoliquiritigenin,sativanone和alpinetin经历了Diels-Alder逆转录裂解。所提出的方法将有助于烟叶的质量控制。

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