Pharmacokinetic Analysis of Four Bioactive Iridoid and Secoiridoid Glycoside Components of Radix Gentianae Macrophyllae and Their Synergistic Excretion by HPLC-DAD Combined with Second-Order Calibration

Natural Products and Bioprospecting, Nov 2017

Tian-Ming Yang, Yang-Xi Liu, Hai-Yan Fu, Wei Lan, Han-Bo Su, He-Bin Tang, Qiao-Bo Yin, He-Dong Li, Li-Ping Wang, Hai-Long Wu

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Pharmacokinetic Analysis of Four Bioactive Iridoid and Secoiridoid Glycoside Components of Radix Gentianae Macrophyllae and Their Synergistic Excretion by HPLC-DAD Combined with Second-Order Calibration

Natural Products and Bioprospecting Pharmacokinetic Analysis of Four Bioactive Iridoid and Secoiridoid Glycoside Components of Radix Gentianae Macrophyllae and Their Synergistic Excretion by HPLC-DAD Combined with Second-Order Calibration Tian-Ming Yang 0 1 Yang-Xi Liu 0 1 Hai-Yan Fu 0 1 Wei Lan 0 1 Han-Bo Su 0 1 He-Bin Tang 0 1 Qiao-Bo Yin 0 1 He-Dong Li 0 1 Li-Ping Wang 0 1 Hai-Long Wu 0 1 0 State Key Laboratory of Chemo/Biosensing and Chemometrics, College of Chemistry and Chemical Engineering, Hunan University , Changsha 410082 , China 1 The Modernization Engineering Technology Research Center of Ethnic Minority Medicine of Hubei Province, School of Pharmaceutical Sciences, South-Central University for Nationalities , Wuhan 430074 , China An HPLC-DAD method combined with second-order calibration based on the alternating trilinear decomposition (ATLD) algorithm with the aid of region selection was developed to simultaneously and quantitatively characterize the synergistic relationships and cumulative excretion of the four bioactive ingredients of Radix Gentianae Macrophyllae in vivo. Although the analytes spectra substantially overlapped with that of the biological matrix, the overlapping profiles between analytes and co-eluting interferences can be successfully separated and accurately quantified by the ATLD method on the basis of the strength of region selection. The proposed approach not only determined the content change but also revealed the synergistic relationships and the cumulative excretion in vivo of the four ingredients in urine and feces samples collected at different excretion time intervals. In addition, several statistical parameters were employed to evaluate the accuracy and precision of the method. Quantitative results were confirmed by HPLC-mass spectrometry. Satisfactory results indicated that the proposed approach can be utilized to investigate the pharmacokinetics of Radix Gentianae Macrophyllae excretion in vivo. Graphical Abstract HPLC-DAD Second-order calibration Pharmacokinetic analysis 1 Introduction Radix Gentianae Macrophyllae belongs to the Gentiana genus of Gentianaceae and is widely used as a remedy in traditional Chinese medicine (TCM) for more than 2000 years [ 1 ]. The dominant bioactive constituents in Radix Gentianae Macrophyllae are iridoid and secoiridoid glycosides, including gentiopicroside (GPS), loganic acid (LOG), swertiamarin (SWM), and sweroside (SWS), which exhibit analgesic, anti-inflammatory, antipyretic, antirheumatic, diuretic, febrifuge, and hypoglycemic pharmacological effects for treating hypotension, rheumatism, pains, fever, and allergic inflammations [ 2–6 ]. Unlike those of chemical drugs, the therapeutic effects of TCM are based on the synergistic effect of their bioactive compounds [ 7 ]. The determination of several components can not sufficiently represent the effects of TCM [ 8 ], whereas multi-component analysis helps reveal the effect of coordination among the TCM components [ 9, 10 ]. Thus, simultaneous quantification of bioactive ingredients in a complex physiological matrix is crucial. Pharmacokinetics describes how the body affects a specific drug after administration through absorption and distribution, the chemical changes of the substance in the body, and the excretion effects and routes of metabolites in the drug [ 11 ]. Pharmacokinetic study on multiple components is a difficult field in TCM research because of the complicated and microscale nature of the chemical components of TCM. Based on the available literature, several analytical methods, such as HPLC-UV [ 12, 13 ], UFLC-MS/MS [14], and LC/MS/MS [ 15 ], are available for quantifying bioactive ingredients derived from Radix Gentianae Macrophyllae in a biological matrix. Chromatographic analysis is an effective strategy to directly determine drugs. However, baseline drift and overlapping of peaks between matrix constituents and compounds of interest often occur in the chromatographic analysis of complex samples. For eliminating the influence of interfering compounds on analytes of interest, complex gradient elution is employed to isolate analytes. Several trivial sample pretreatments and instrumental parameters require optimization, entailing considerable energy, time, and cost. Second-order calibration is widely used in numerous scientific areas, such as food quality and safety [ 16–24 ], cosmetic research [ 25, 26 ], environmental monitoring [ 27–30 ], biochemical assay [ 31–37 ], and routine analysis [ 38–40 ]. The strategy is a good solution to the previously mentioned problems because the concentrations of individual components can be accurately obtained even in the presence of uncalibrated interferences, that is, ‘‘secondorder advantage.’’ Pharmacokinetic research on TCM is always performed using chromatographic technique, which offers advantages of powerful separation and analysis capabilities. However, an extremely complex gradient (...truncated)


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Tian-Ming Yang, Yang-Xi Liu, Hai-Yan Fu, Wei Lan, Han-Bo Su, He-Bin Tang, Qiao-Bo Yin, He-Dong Li, Li-Ping Wang, Hai-Long Wu. Pharmacokinetic Analysis of Four Bioactive Iridoid and Secoiridoid Glycoside Components of Radix Gentianae Macrophyllae and Their Synergistic Excretion by HPLC-DAD Combined with Second-Order Calibration, Natural Products and Bioprospecting, 2017, pp. 445-459, Volume 7, Issue 6, DOI: 10.1007/s13659-017-0145-7