Optimization of an extraction method for the simultaneous quantification of sixteen polyphenols in thirty-one pulse samples by using HPLC-MS/MS dynamic-MRM triple quadrupole

Caprioli, Giovanni; Nzekoue, Franks Kamgang; Giusti, Federica; Vittori, Sauro; Sagratini, Gianni

doi:10.1016/j.foodchem.2018.06.049

Cited by 29 publications

(19 citation statements)

References 23 publications

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“…This is in agreement with the minimal matrix effects in various complex bio-matrices as reported by Hurtado-Gaitán et al, who focused on grapevine stilbcncs while employing a similar state-of-the-art analytical instrument as ours [33]. Ion suppression of a few phenolic compounds was however observed by Caprioli et al also using the advanced analytical instrumentation but this was likely due to the high protein and carbohydrate content found in their pulse extracts [34]. Overall, the holistic performance of the extraction process and LC-MS method should be considered satisfactory, and analyses of biological samples containing the broth matrix were not affected by the matrix effect.…”

Section: Resultssupporting

confidence: 88%

Development and validation of an ultra-high performance liquid chromatography/triple quadrupole mass spectrometry method for analyzing microbial-derived grape polyphenol metabolites

Zhao

Yuan

Carry

et al. 2018

Journal of Chromatography B

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Accumulating evidence indicates that the health impact of dietary phenolic compounds, including the principal grape-derived polyphenols, (+)‑catechin and (-)‑epicatechin, is exerted by not only the parent compounds but also their phenolic metabolites generated by the gut microbiota. In this work, a new high-throughput, sensitive and reproducible analytical method was developed employing ultra-high performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry (UHPLC-QqQ-MS/MS) for the simultaneous analysis of 16 microbial-generated phenolic acid metabolites (PAMs) along with their precursors, catechin and epicatechin. Following optimizing the solvent system, LC conditions and MS parameters, method validation was carried out to evaluate the sensitivity, selectivity, accuracy and precision of the proposed method, and to ensure promising recovery of all analytes extracted from the matrix prior to bioanalysis. Results showed that the optimized analytical method allowed successful confirmation and quantitation of all analytes under dynamic multiple reaction monitoring mode using trans‑cinnamic acid‑d as an internal standard (I.S.). Excellent sensitivity and linearity were obtained for all analytes, with lower limits of detection (LLODs) and lower limits of quantification (LLOQs) in the ranges of 0.225-2.053 ng/mL and 0.698-8.116 ng/mL, respectively. By examining blank matrix spiked with standard mixture at different concentration levels, promising recoveries at two spiking levels (low level, 91.2-115%; high level 90.2-121%), and excellent precision (RSD < 10%) were obtained. This method was then successfully applied to an in vitro study where catechin/epicatechin-enriched broth samples were anaerobically fermented with gut microbes procured from healthy human donors. All sources of bacteria employed showed remarkable activity in metabolizing grape polyphenols and distinct variations in the production of PAMs. The successful application of this method in the in vitro fermentation assays demonstrates its suitability for high-throughput analysis of polyphenol metabolites, particularly catechin/epicatechin-derived PAMs, in biological studies.

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Section: Resultssupporting

confidence: 88%

Development and validation of an ultra-high performance liquid chromatography/triple quadrupole mass spectrometry method for analyzing microbial-derived grape polyphenol metabolites

Zhao

Yuan

Carry

et al. 2018

Journal of Chromatography B

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“…Therefore, Method 4, i.e., an ethanol/water (70/30) extraction assisted by sonication, was the best procedure in term of extraction efficiency not only for caffeine and chlorogenic acids but also for polyphenols. This solvent was the best for the extraction of sixteen polyphenols from pulse samples as well [ 43 ]. Interesting levels of polyphenols were also obtained when the extraction was performed under acid condition (Method 5).…”

Section: Resultsmentioning

confidence: 99%

“…Interesting levels of polyphenols were also obtained when the extraction was performed under acid condition (Method 5). This could be due to the prevention of polyphenols oxidation at low pH [ 43 ].…”

Section: Resultsmentioning

confidence: 99%

Characterization of Odor-Active Compounds, Polyphenols, and Fatty Acids in Coffee Silverskin

et al. 2020

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For the first time the volatile fraction of coffee silverskin has been studied focusing on odor-active compounds detected by gas chromatography-olfactometry/flame ionization detector (GC-O/FID) system. Two approaches, namely headspace (HS) analysis by solid-phase microextraction-gas chromatography-mass spectrometry (SPME-GC-MS) and odor-active compounds analysis by gas chromatography-olfactometry/flame ionization detector (GC-O/FID), have been employed to fully characterize the aroma profile of this by-product. This work also provided an entire characterization of the bioactive compounds present in coffee silverskin, including alkaloids, chlorogenic acids, phenolic acids, flavonoids, and secoiridoids, by using different extraction procedures and high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) system. Coffee silverskin was shown to be a good source of caffeine and chlorogenic acids but also of phenolic acids and flavonoids. In addition, the fatty acid composition of the coffee silverskin was established by GC-FID system. The results from this research could contribute to the development of innovative applications and reuses of coffee silverskin, an interesting resource with a high potential to be tapped by the food and nutraceutical sector, and possibly also in the cosmetics and perfumery.

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“…In this manner, analytes were only monitored while they were eluting from the LC, and MS did not waste time by monitoring them when they were not expected. 28 spiking levels, for already studied molecules in coffee, was chosen according to literature data 27,35 and for others according to the contents found in blank samples. The standard solution was added before the extraction process (prespike) and, in a second experiment, after the extraction process (post spike).…”

Section: Optimization Of the Hplc-ms/ms Analytical Methodsmentioning

confidence: 99%

An analytical method for the simultaneous quantification of 30 bioactive compounds in spent coffee ground by HPLC‐MS/MS

et al. 2020

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Spent coffee ground (SCG) is the remaining residue produced after extraction of coffee, and it is considered a source of unextracted bioactive compounds. For this, in the latest years, the attention has been focused to innovative reuses that can exploit the potentiality of SCG. Unfortunately, the content of bioactive compounds has not been thoroughly studied yet, and the major of publication has investigated the caffeine and chlorogenic acids levels, total polyphenol contents, and total flavonoid content. Hence, these approaches have determined only an estimation of flavonoids and polyphenols content and lack on single polyphenols investigation. Therefore, the objective of the current work was to provide a deep characterization of bioactive compounds in SCG. For this purpose, a new analytical method for the quantification of 30 molecules, including caffeine, chlorogenic acids, phenolic acids, flavonoids, and secoiridoids, has been developed using high-performance liquid chromatography tandem mass spectrometry. Moreover, several extraction procedures, that is, liquid-solid extraction assisted and not by ultrasounds, testing diverse solvents, were evaluated. Liquid-solid extraction assisted by sonication, with water/ethanol (30/70, v/v), resulted the best in terms of total bioactive compounds, and, once validated, the new analytical method was applied to five different espresso SCG samples. Data showed that caffeine (means: 1193.886 ± 57.307 mg kg −1) and chlorogenic acids (means of total CQAs: 1705.656 ± 88.694 mg kg −1) were the most abundant compounds in all SCG samples followed by phenolic acids such as caffeic, ferulic, gallic, p-coumaric, syringic, trans-cinnamic, and vanillic acid. Moreover, some flavonoids, that is, rutin, cyanidin 3-glucoside, and quercetin, occurred in almost all samples. This work provided a deepened characterization of bioactive compounds in SCG and can contribute to develop new strategies of reuses.

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Optimization of an extraction method for the simultaneous quantification of sixteen polyphenols in thirty-one pulse samples by using HPLC-MS/MS dynamic-MRM triple quadrupole

Cited by 29 publications

References 23 publications

Development and validation of an ultra-high performance liquid chromatography/triple quadrupole mass spectrometry method for analyzing microbial-derived grape polyphenol metabolites

Development and validation of an ultra-high performance liquid chromatography/triple quadrupole mass spectrometry method for analyzing microbial-derived grape polyphenol metabolites

Characterization of Odor-Active Compounds, Polyphenols, and Fatty Acids in Coffee Silverskin

An analytical method for the simultaneous quantification of 30 bioactive compounds in spent coffee ground by HPLC‐MS/MS

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