Determination of Miroestrol and Isomiroestrol From Pueraria mirifica (White Kwao Krua) in Dietary Supplements by LC-MS-MS and LC-Q-Orbitrap/MS
Determination of Miroestrol and Isomiroestrol From Pueraria mirifica (White Kwao Krua) in Dietary Supplements by LC-MS-MS and LC-Q-Orbitrap/MS
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DOI：
10.1093/chromsci/bmw171
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发表时间：
2017-03-01
影响因子：
1.3
通讯作者：
Baek, Sun Young
中科院分区：
文献类型：
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作者：
Lee, Ji Hyun;Kim, Jung Yeon;Baek, Sun Young
本研究旨在建立液相色谱-串联质谱（LC-MS-MS）和液相色谱-Q-轨道阱/质谱（LC-Q-Orbitrap/MS）联用技术分析葛根中违禁成分的方法。空白样品和加标miroestrol和isomiroestrol的样品用于初始开发和验证研究。采用专属性、线性、定量限（LOQ）、检测限（LOD）、准确度、精密度、回收率和稳定性作为验证参数。发现miroestrol和isomiroestrol的LOD分别为4.17和0.84 ng/mL，而它们的LOQ分别为12.50和2.52 ng/mL。日内和日间精密度分别为0.8- 6.9%和1.9- 9.8%，日内和日间准确度分别为82.1- 103.7%和85.0- 109.7%。从膳食补充剂的目标化合物的平均回收率范围为86.9%至108.9%。回收率的相对标准偏差（RSD）为
The purpose of this study is to develop LC-MS-MS and LC-Q-Orbitrap/MS method for the analysis of the components of Pueraria mirifica, which are illegal additives in dietary supplements. Blank samples and samples spiked with miroestrol and isomiroestrol were used for the initial development and validation studies. Specificity, linearity, limit of quantification (LOQ), limit of detection (LOD), accuracy, precision, recovery and stability were employed as the validation parameters. The LODs of miroestrol and isomiroestrol were found to be 4.17 and 0.84 ng/mL, respectively, whereas their LOQs were 12.50 and 2.52 ng/mL, respectively. The determination coefficient was over 0.999, intra- and inter-day precisions were 0.8-6.9 and 1.9-9.8%, respectively, and intra and inter-day accuracies were 82.1-103.7 and 85.0-109.7%, respectively. The mean recoveries of the targeted compounds from the dietary supplements ranged from 86.9 to 108.9%. The relative standard deviations (RSDs) for recovery were