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HPLC-MS/MS 测定皂刺中黄酮类化合物的含量,用于其质量评估。

HPLC-MS/MS determination of flavonoids in Gleditsiae Spina for its quality assessment.

机构信息

Shenzhen Institute for Drug Control, Shenzhen, P. R. China.

Shenzhen Key Laboratory of Drug Quality Standard Research, Shenzhen, P. R. China.

出版信息

J Sep Sci. 2018 Apr;41(8):1752-1763. doi: 10.1002/jssc.201701249. Epub 2018 Feb 1.

Abstract

Gleditsiae Spina, the thorn of Gleditsia sinensis Lam., has been used as an anti-inflammatory, anti-tumor, and anti-bacterial traditional medicine for hundreds of years in China. This study used high-performance liquid chromatography and tandem mass spectrometry combined with chemometric methods to allow the fast and accurate identification and quantification of the flavonoids compounds in Gleditsiae Spina, and created reliable criteria for accurate identification of Gleditsiae Spina and its adulterants. This research provides good evidence for the classification and quality evaluation of Gleditsiae Spina. Firstly, eight flavonoids compounds were detected and identified on the basis of their mass spectra, fragment characteristics, and comparison with published data. Then the mass spectroscopic fragmentation pathways of these compounds were determined and, in addition rutin, isoquercitrin, and quercitrin were detected in Gleditsiae Spina for the first time. The quantification was performed on a triple quadrupole tandem mass spectrometer in multi-reaction monitoring mode, and the baseline separation of the eight bioactive flavonoids components was achieved within 13 min. Furthermore, the proposed method was successfully applied for simultaneous quantitative determination of the eight Gleditsiae Spina compounds and adulterants obtained from different sources in China. Then, we built a classification model which showed a high level of accuracy predicting 100% of the samples, correctly.

摘要

皂荚刺,即皂荚的棘刺,在中国已被用作抗炎、抗肿瘤和抗菌的传统药物数百年。本研究采用高效液相色谱-串联质谱联用结合化学计量学方法,快速准确地鉴定和定量分析了皂荚刺中的黄酮类化合物,并为准确鉴定皂荚刺及其掺杂物创建了可靠的标准。该研究为皂荚刺的分类和质量评价提供了良好的证据。首先,在基于质谱、碎片特征和与已发表数据的比较的基础上,检测并鉴定了 8 种黄酮类化合物。然后确定了这些化合物的质谱裂解途径,此外首次在皂荚刺中检测到芦丁、异槲皮苷和槲皮苷。采用三重四极杆串联质谱在多反应监测模式下进行定量分析,在 13 分钟内实现了 8 种生物活性黄酮类成分的基线分离。此外,该方法还成功应用于同时定量测定来自中国不同来源的 8 种皂荚刺化合物及其掺杂物。然后,我们建立了一个分类模型,该模型对 100%的样本具有很高的预测准确性。

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