Application of FTIR Spectroscopy and HPLC Combined with Multivariate Calibration for Analysis of Xanthones in Mangosteen Extracts

Abstract

Mangosteen, or Garcinia mangostana L., has merged as an emerging fruit to be investigated due to its active compounds, especially xanthone derivatives such as α -mangostin (AM), γ-mangostin (GM), and gartanin (GT). These compounds had been reported to exert some pharmacological activities, such as antioxidant and anti-inflammatory, therefore, the development of an analytical method capable of quantifying these compounds should be investigated. The aim of this study was to determine the correlation between FTIR spectra and HPLC chromatogram, combined with chemometrics for quantitative analysis of ethanolic extract of mangosteen. The ethanolic extract of mangosteen pericarp was prepared using the maceration technique, and the obtained extract was subjected to measurement using instruments of FTIR spectrophotometer at wavenumbers of 4000–650 cm−1 and HPLC, using a PDA detector at 281 nm. The data acquired were subjected to chemometrics analysis of partial least square (PLS) and principal component regression (PCR). The result showed that the wavenumber regions of 3700–2700 cm−1 offered a reliable method for quantitative analysis of GM with coefficient of determination (R2) 0.9573 in calibration and 0.8134 in validation models, along with RMSEC value of 0.0487% and RMSEP value 0.120%. FTIR spectra using the second derivatives at wavenumber 3700–663 cm−1 with coefficient of determination (R2) >0.99 in calibration and validation models, along with the lowest RMSEC value and RMSEP value, were used for quantitative analysis of GT and AM, respectively. It can be concluded that FTIR spectra combined with multivariate are accurate and precise for the analysis of xanthones.

α-Mangostin/γ-Cyclodextrin Inclusion Complex: Formation and Thermodynamic Study

“…The strong band at 3000–3500 cm −1 corresponds to the hydrogen bond of the hydroxyl groups. The weak absorption 2930 cm −1 corresponds with the methylene (CH 2 ) groups, 1640 cm −1 is given by CH 3 bending, 998 cm −1 is the bend absorption of C-OH stretching vibration, and 598 cm −1 indicates –CH=CH- bending [ 34 , 35 ].…”

“…This phenomenon was previously reported about the complex formation of budenoside/γ-CD. The last study findings suggest that cogrinding and coprecipitation resulted in the formation of an inclusion complex and that this influenced the particle diameter and particle surface [ 34 ]. Our study found that the crystallinity of α-M/γ-CD CX was 28.2%, while the intact α-M and γ–CD were 91.1% and 62.6%, respectively.…”

“…The absorption bands at 1580 cm , 1645 cm −1 , and 1630 cm −1 are the stretching vibrations of unconjugated C=C in α-M. The band at 1470 cm −1 is given by the unconjugated carbonyl group (C=O) on the B ring of α-M; 1362 cm −1 is given by CH3 bending; 1083 cm −1 and 1051 cm −1 correspond with the stretching vibration of C-O; and 1011 cm −1 , 862 cm −1 , 804 cm −1 , 772 cm −1 , and 598 cm −1 are given by C-OH stretching, -CH=CH-(trans), -CH=CH-(cis), CH2, and -CH=CH-bending, respectively [34]. The second graph (γ-CD) shows a broad absorption around 3000-3600 cm −1 with a maximum absorption at 3395 cm −1 .…”

“…A high-intensity doublet, with maximum absorption at 1030 cm −1 and 1000 cm −1 , is assigned to the C-H out-of-plane bending vibrations and the C-OH stretching vibration modes, respectively. The band at 598 cm −1 is given by -CH=CH-bending [34,35]. The FTIR spectra of α-M, γ-CD, α-M/γ-CD PM, and α-M/γ-CD CX are shown in Figure 3.…”

Implementation of chemometrics as a Solution to detecting and preventing falsification of herbal medicines in Southeast Asia: A review

“…The study conducted by Tejamukti et al (2020) reveals that xanthone derivate contents can be determined using FTIR combined multivariate calibration of PLSR and PCR. Like flavonoids, a xanthone derivate also has various biological activities among others (Rivero and Garibay, 2019), such as antioxidant, analgesic, anti-inflammatory, antifungal, and anthelmintic activities (El-Kenawy et al, 2018).…”