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化学计量学结合 UPLC-MS/MS 同时分析生、炒葶苈子中的指标成分,并应用 Box-Behnken 设计优化炮制工艺。

Chemometrics coupled with UPLC-MS/MS for simultaneous analysis of markers in the raw and processed Fructus Xanthii, and application to optimization of processing method by BBD design.

机构信息

Key Laboratory of Chinese Materia Medica, Heilongjiang University of Chinese Medicine, Ministry of Education, Harbin 150040, PR China.

Key Laboratory of Chinese Materia Medica, Heilongjiang University of Chinese Medicine, Ministry of Education, Harbin 150040, PR China; School of Traditional Chinese Medicine, Guangdong Pharmaceutical University, Guangzhou 528458, PR China.

出版信息

Phytomedicine. 2019 Apr;57:191-202. doi: 10.1016/j.phymed.2018.12.020. Epub 2018 Dec 15.

DOI:10.1016/j.phymed.2018.12.020
PMID:30776590
Abstract

BACKGROUND

As a widely used toxic traditional herbal medicine, the quality of the Fructus Xanthii must be well controlled to ensure the clinical therapeutic efficacy and safety.

AIMS

A rapid, and sensitive using ultra-high performance liquid chromatography to triple quadrupole tandem mass spectrometry (UPLC-MS/MS) in selected reaction monitoring (SRM) mode was developed and validated for simultaneous quantitation of determination active and toxic ingredients form processed by stir-frying and raw materials of Fructus Xanthii.

METHODS

Chromatographic separation of all targeted compound was performed on Waters ACQUITY UPLC HSS T3 column (50 mm × 2.1 mm, 1.8 μm). Moreover, the method was successfully applied in thirty-six samples of Fructus Xanthii collected from different sources in China. The processing method was optimized through Box-Behnken statistical design and response surface methodology.

RESULTS

In this work, chemometrics was able to successfully discriminate and classify among samples. The optimal incubation conditions were as follows: under heating in a pot at 295 °C, medicine at 120 °C for 11.0 min with flipping frequently.

CONCLUSIONS

Therefore, the established UPLC-QQQ-MS method in combination with chemometric analysis provides a rapid, flexible and reliable method for quality assessment of Fructus Xanthii. Importantly, the optimized experimental value of the processing process provides the basis for future research.

摘要

背景

作为一种广泛使用的有毒传统草药,必须对葶苈子的质量进行良好的控制,以确保其临床疗效和安全性。

目的

建立一种快速、灵敏的超高效液相色谱-三重四极杆串联质谱法(UPLC-MS/MS),采用选择反应监测(SRM)模式,同时定量测定炒葶苈子和葶苈子生品的活性和毒性成分。

方法

采用 Waters ACQUITY UPLC HSS T3 柱(50mm×2.1mm,1.8μm)进行所有目标化合物的色谱分离。此外,该方法还成功应用于中国不同来源的 36 份葶苈子样品。通过 Box-Behnken 统计设计和响应面法对炮制方法进行了优化。

结果

在本研究中,化学计量学能够成功地对样品进行区分和分类。最佳的孵化条件如下:在锅中加热至 295℃,频繁翻动,药物在 120℃下加热 11.0 分钟。

结论

因此,建立的 UPLC-QQQ-MS 法结合化学计量学分析为葶苈子的质量评估提供了一种快速、灵活、可靠的方法。重要的是,该炮制工艺的优化实验值为今后的研究提供了依据。

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