Quality Control

Determination of two alkaloids in Quisqualis Fructus Semen by UHILIC-MS/MS and NIRS method*

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  • 1. College of Pharmacy, Fujian University of Traditional Chinese Medicine, Fuzhou 350122, China;
    2. Fujian Institute for Food and Drug Quality Control, Fuzhou 350001, China

Received date: 2023-03-17

  Online published: 2024-06-25

Abstract

Objective: To establish an ultra hydrophilic interaction chromatography-tandem mass spectrometry (UHILIC-MS/MS) for the simultaneous determination of trigonelline and quisqualic acid in Quisqualis Fructus Semen, then the rapid quantitative model of near infrared spectroscopy (NIRS) was established for the quality control of Quisqualis Fructus Semen. Methods: The UHILIC-MS/MS assay was performed on a Waters ACQUITY BEH HILIC Amide (2.1 mm×100 mm,1.7 μm) column with 0.1% formic acid aqueous (A)-acetonitrile (B) as mobile phase by gradient elution at a flow rate of 0.20 mL·min-1, and the column temperature was set at 45 ℃. Positive and negative electrospray ionization were performed in multiple reaction monitoring (MRM) mode. The NIRS of Quisqualis Fructus Semen powder was obtained with a resolution of 10 cm-1 in the wavelength range of 100 0-179 9 nm. The collection method was diffuse reflection, and the quantitative models of these two components were constructed by partial least squares (PLS). Results: Under the UHILIC-MS/MS method, trigonelline and quisqualic acid showed good linear relationships within their tested ranges, which were 5.20-260 and 8.50-425 ng·mL-1, respectively (r>0.999 3). The recoveries of trigonelline and quisqualic acid were 101.55% and 100.16%, and RSDs were 1.3% and 2.0%, respectively. There was a good linear relationship between the NIRS predicted values of trigonelline and quisqualic acid and the UHILIC-MS/MS measured values (R>0.976 9). The corrected correlation coefficients (Rc) were 0.977 0 and 0.971 8, the predictive correlation coefficient (Rp) were 0.955 3 and 0.946 4, the calibration set cross-validation root mean square error (RMSEC) were 0.373 9 and 0.284 8, and the root square error of prediction (RMSEP) were 0.490 2 and 0.363 5, respectively. Then the model was validated by 10 batches of Quisqualis Fructus Semen samples beyond the established model, and the average relative deviation of the NIRS predictive value and measured values were 0.242% and 0.252%, respectively. Conclusion: It is the first report about simultaneous analysis of trigonelline and quisqualic acid in Quisqualis Fructus Semen by using UHILIC-MS/MS method, which affords fast and efficient method for the content determination of two alkaloids in Quisqualis Fructus Semen. It is also the first time to establish determination of trigonelline and quisqualic acid by NIRS quantitative model. The model is proved to be efficient and accurate, which provides a new and feasible method for the rapid quality evaluation of Quisqualis Fructus Semen.

Cite this article

WANG Li-na, ZHANG Ying, WEN Xiu-ping, XU Wei, YU Bo, XU Wen, LIN Yu, CHEN Zai-min . Determination of two alkaloids in Quisqualis Fructus Semen by UHILIC-MS/MS and NIRS method*[J]. Chinese Journal of Pharmaceutical Analysis, 2023 , 43(6) : 999 -1011 . DOI: 10.16155/j.0254-1793.2023.06.11

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