Simultaneous Determination of 19 Bioactive Constituents in QishenYiqi Dropping Pills by Ultra-Performance Liquid Chromatography Coupled with Triple Quadrupole Mass Spectrometry

2019 ◽  
Vol 102 (4) ◽  
pp. 1102-1111 ◽  
Author(s):  
Qingling Xie ◽  
Hanwen Yuan ◽  
Yongbei Liu ◽  
Yixing Qiu ◽  
Yuqing Jian ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Salvia Miltiorrhiza ◽  
Panax Notoginseng ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Scientific Basis ◽  
Triple Quadrupole ◽  
Bioactive Constituents ◽  
High Definition

Abstract Background: QishenYiqi dripping pills (QSYQ), consisting of Salvia miltiorrhiza, Astragalus membranaceus, Panax notoginseng, and Dalbergia odorifera, is a widely used to treat ischemic cerebrovascular and hemorrhagic cerebrovascular in China. Objective: In this study, a rapid and sensitive ultra-HPLC coupled with a triple quadrupole MS (UHPLC-QQQ-MS) method was established for the simultaneous quantification of 19 bioactive components. Methods: Chromatographic separation was performed on an Agilent Eclipse Plus C18 Rapid Resolution High Definition (RRHD) column (2.1 × 50 mm, 1.8 μm) with a mobile phase composed of a 0.1% (v/v) formic acid aqueous solution and acetonitrile in a gradient elution manner. A QQQ-MS was used in positive and negative ionization mode with multiple reactions monitoring for quantitative analysis. Results: The established methods were validated with linearity, precision, repeatability, stability, recovery, and matrix effect. All calibration curves exhibited excellent linear relationship with the correlation coefficient (r) >0.9985 for each analyte within the test range. This method was successfully applied to quantify target compounds of different structural types in 12 batches of QSYQ. Conclusions: The results suggest that the established method is rapid, sensitive, and reliable. The developed UHPLC-QQQ-MS method can provide scientific basis and reference to quality control and consistency evaluation of QSYQ sample and other formulations. Highlights: A rapid, sensitive, and reliable UHPLC-QQQ-MS method has been developed and validated for simultaneous determination of 19 compounds including phenolic acids, saponins, isoflavonoids, and tanshinones in QSYQ for the first time.

Simultaneous determination of eight ginsenosides in Zibu Piyin Recipe using ultra-performance liquid chromatography coupled with triple-quadrupole mass spectrometry (UPLC-MS/MS)

2015 ◽  
Vol 7 (18) ◽  
pp. 7527-7533
Author(s):  
Hui-Ying Xu ◽  
Hong Xiang ◽  
Li-Bin Zhan ◽  
Lin Zhang ◽  
Xiao-Xin Sun
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Simultaneous Determination ◽  
Simultaneous Detection ◽  
Ultra Performance Liquid Chromatography ◽  
Triple Quadrupole ◽  
Quadrupole Mass ◽  
Quadrupole Mass Spectrometry ◽  
Detection And Quantification

A simple, sensitive, selective, and reliable UPLC-MS/MS method was developed and validated for the simultaneous detection and quantification of eight compounds found in Zibu Piyin Recipe (ZBPYR).

A Rapid and Accurate 1HNMR Method for the Identification and Quantification of Major Constituents in Qishen Yiqi Dripping Pills

2020 ◽  
Author(s):  
Qingling Xie ◽  
Limin Gong ◽  
Feibing Huang ◽  
Mengru Cao ◽  
Yongbei Liu ◽  
...  
Keyword(s):  
Simultaneous Determination ◽  
Chemical Shifts ◽  
Salvia Miltiorrhiza ◽  
Proton Nmr ◽  
Herbal Medicines ◽  
Panax Notoginseng ◽  
Hplc Method ◽  
Coupling Constants ◽  
Identification And Quantification

Abstract Background Qishen Yiqi dripping pills (QSYQ), composed of four herbal medicines—Salvia miltiorrhiza, Astragalus membranaceus, Panax notoginseng, and Dalbergiaodorifera—are widely used to treat ischemic cerebrovascular and hemorrhagic cerebrovascular conditions. Objective In this study, a rapid and accurate proton NMR (1HNMR) spectroscopy method was established to control the quality of QSYQ and ensure their clinical efficacy. Method Firstly, different types of metabolites were identified based on the proton signal peaks of chemical shifts, coupling constants, and related information provided through two-dimensional NMR spectroscopy. Secondly, a quantitative 1HNMR method was established for the simultaneous determination of major constituents in QSYQ samples. In addition, an HPLC method was performed to verify the results obtained by the quantitative proton NMR (qHNMR)  method. Results In the present study, 26 metabolites were identified in the 1HNMR spectra of QSYQ. In addition, a rapid and accruate qHNMR method was established for the simultaneous determination of protocatechualdehyde, rosmarinic acid, danshensu, calycosin-7-O-β-D-glucoside, and ononin in ten batches of QSYQ samples for the first time. Moreover, the proposed qHNMR method and HPLC method were compared using Bland-Altman and plots Passing-Bablok regression, indicating no significant differences and a strong correlation between the two analytical methods. Conclusions This method is an important tool for the identification and quantification of major constituents in QSYQ. Highlights Compared with traditional HPLC, the established qHNMR method has the advantages of simple sample preparation, short analysis time, and non-destructive analysis.

scholarly journals A Validated UPLC-PDA Method for Simultaneous Determination of 3 Biologically Active Isoflavans in Trigonella stellata Extract

2020 ◽  
Vol 15 (7) ◽  
pp. 1934578X2094011
Author(s):  
Safa M. Shams Eldin ◽  
Mohamed M. Radwan ◽  
Amira S. Wanas ◽  
Abdel-Azim M. Habib ◽  
Fahima F. Kassem ◽  
...  
Keyword(s):  
Formic Acid ◽  
Simultaneous Determination ◽  
Correlation Coefficients ◽  
Gradient Elution ◽  
Ultra Performance Liquid Chromatography ◽  
Biologically Active ◽  
External Standard Method ◽  
Acid Aqueous Solution ◽  
Acquity Uplc

In this study, an ultra-performance liquid chromatography (UPLC)/photodiode array method was developed for the simultaneous determination of trigonellan glucoside (1), isotrigonellan (2), and methoxy-isotrigonellan (3) in Trigonella stellata extract using an external standard method. The extract was prepared using a standardized method by maceration of the dried plant material in ethanol. The 3 isoflavans (1-3) were separated on an Acquity UPLC C18 column using gradient elution with a mobile phase consisting of 0.1% (v/v) formic acid aqueous solution and 0.1% (v/v) formic acid in acetonitrile, and ultraviolet detection. The method provides a linear correlation for all analytes over the investigated ranges with all correlation coefficients greater than 0.998. The validated lower limits of quantitation were 53, 127, and 5 μg/mL for isoflavans 1, 2, and 3, respectively. Intraday and interday precisions (percent relative SD [RSD%]) were less than 8.3% and accuracy (RE%) ranged from 90% to 100%. The method’s capability to remain unaffected by small, but deliberate variations in method parameters (method’s reliability during normal usage) described by the robustness showed RSD% less than 4.6% measured by varying 3 different parameters. The validated method was successfully applied to simultaneously determine the concentration of the 3 new isoflavans having anti-inflammatory and antidiabetic activities. The results revealed that the validated method can be used for quality control of herbal preparations containing these or similar isoflavans that are marketed for the prevention of inflammation and as antidiabetics.

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