Abstract

Chemical profiling of Buddleja globosa was performed by high-performance liquid chromatography coupled to electrospray ionization (HPLC-DAD-ESI-IT/MS) and quadrupole time-of-flight high-resolution mass spectrometry (HPLC-ESI-QTOF/MS). The identification of 17 main phenolic compounds in B. globosa leaf extracts was achieved. Along with caffeoyl glucoside isomers, caffeoylshikimic acid and several verbascoside derivatives (β-hydroxyverbascoside and β-hydroxyisoverbascoside) were identified. Among flavonoid compounds, the presence of 6-hydroxyluteolin-7-O-glucoside, quercetin-3-O-glucoside, luteolin 7-O-glucoside, apigenin 7-O-glucoside was confirmed. Campneoside I, forsythoside B, lipedoside A and forsythoside A were identified along with verbascoside, isoverbascoside, eukovoside and martynoside. The isolation of two bioactive phenolic compounds verbascoside and forsythoside B from Buddleja globosa (Buddlejaceae) was successfully achieved by centrifugal partition chromatography (CPC). Both compounds were obtained in one-step using optimized CPC methodology with the two-phase solvent system comprising ethyl acetate-n-butanol-ethanol-water (0.25:0.75:0.1:1, v/v). Additionally, eight Natural Deep Eutectic Solvents (NADESs) were tested for the extraction of polyphenols and compared with 80% methanol. The contents of verbascoside and luteolin 7-O-glucoside after extraction with 80% methanol were 26.165 and 3.206 mg/g, respectively. Among the NADESs tested in this study, proline- citric acid (1:1) and choline chloride-1, 2- propanediol (1:2) were the most promising solvents. With these NADES, extraction yields for verbascoside and luteolin 7-O-glucoside were 51.045 and 4.387 mg/g, respectively. Taken together, the results of this study confirm that CPC enabled the fast isolation of bioactive polyphenols from B. globosa. NADESs displayed higher extraction efficiency of phenolic and therefore could be used as an ecofriendly alternative to classic organic solvents.

Highlights

  • Buddleja globosa Hope (Buddlejaceae) is a native species cultivated in Chile, Peru and Argentina

  • To the best of our knowledge, caffeoylglucoside isomers, caffeoylshikimic acid, β-hydroxy-verbascoside, β-hydroxyisoverbascoside, quercetin-3-O-glucoside, campneoside I, forsythoside B, lipedoside A, forsythoside A, eukovoside and martynoside were identified for the first time in B. globosa using liquid chromatography coupled with IT and time-of flight (TOF)

  • Our features indicate that the strategy of coupling liquid chromatography (LC) with ion trap mass spectrometry (IT-MS) and time-of-flight mass spectrometry (TOF-MS) is a powerful tool for the qualitative analysis of complex samples

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Summary

Introduction

Buddleja globosa Hope (Buddlejaceae) is a native species cultivated in Chile, Peru and Argentina. In the previous work of Backhouse et al [9] matico leaves were extracted with solvents of increasing polarity to obtain different fractions. The separation techniques that have been used to determine phenolic compounds in Buddleja globosa were namely, gas chromatography (GC) and high-performance liquid chromatography (HPLC), all coupled to different detection systems [11,12]. The isolation of bioactive compounds from B. globosa has been performed by conventional extraction techniques [9,16] using organics solvents such as alcohols, chloroform and ethyl acetate. Some of these organic solvents are often toxic, flammable, explosive, and poorly biodegraded. Pounds naamndelyt,oveevrbaaluscaotseidteheanfdeafsoirbsiyltihtyosoidfeeiBghustindgiffceernetnritfuNgaAl DCEPCSspfaorrtittihoen ecxhtrroa-ction of bioactive matographcyom(CpPoCu)nadnsdftroomevaBl.ugaltoebtohsea fceoamsibpilairtyedofweiitghht80d%iffemreentthNanAoDl.ESs for the extraction of bioactive compounds from B. globosa compared with 80% methanol

Results and Discussion
Chloroform- n-butanol-methanol-water
Instruments and Chromatographic Conditions
Q-TOF High-Resolution Mass Spectrometry Measurements
Preparation of NADES
Statistical Analysis
Conclusions
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