Dataset Information

Simultaneous Quantification of Antioxidant Compounds in Phellinus igniarius Using Ultra Performance Liquid Chromatography-Photodiode Array Detection-Electrospray Ionization Tandem Mass Spectrometry.

ABSTRACT: Natural antioxidants are widely used in the life sciences. Phellinus igniarius is a historically used natural antioxidant containing a variety of active compounds. Phenols, particularly Inoscavin A and Hypholomine B, are found in the high concentrations. Better quantitative methods are needed to perform quality control in order to support further research of this mushroom. An ultra-performance liquid chromatography method coupled to photodiode-array detection and an electrospray ionization tandem mass spectrometry method (UPLC-PAD-MS) was developed to simultaneously quantify Inoscavin A and Hypholomine B levels in the medicinal fungus Phellinus igniarius. The two compounds were quantified using UPLC-PAD and UPLC-MS. The methods were accurate (mean accuracy for spiked matrix ranged from 101.5% to 105.8%), sensitive (limit of detection ranged from 0.28 to 1.14 mg L-1) and precise (the relative standard deviations ranged from 0.13 to 2.8%). Inoscavin A and Hypholomine B were purified using high-speed counter-current chromatography (HSCCC), structural evaluated to meet the request of standard substances. UPLC separation was performed on a reversed-phase C18 column using gradient elution with acetonitrile and 0.1% formic acid over 10 min. The developed method was successfully applied to determine Inoscavin A and Hypholomine B in twelve Phellinus igniarius samples of different origins and the results showed that it was suitable for the analysis of these active components in Phellinus igniarius samples.

SUBMITTER: Shou D

PROVIDER: S-EPMC5045194 | biostudies-literature | 2016

REPOSITORIES: biostudies-literature

ACCESS DATA

Publications

Simultaneous Quantification of Antioxidant Compounds in Phellinus igniarius Using Ultra Performance Liquid Chromatography-Photodiode Array Detection-Electrospray Ionization Tandem Mass Spectrometry.

Shou Dan D Dong Yu Y Wang Nani N Li Hongyu H Zhang Yang Y Zhu Yan Y

PloS one 20160930 9

Natural antioxidants are widely used in the life sciences. Phellinus igniarius is a historically used natural antioxidant containing a variety of active compounds. Phenols, particularly Inoscavin A and Hypholomine B, are found in the high concentrations. Better quantitative methods are needed to perform quality control in order to support further research of this mushroom. An ultra-performance liquid chromatography method coupled to photodiode-array detection and an electrospray ionization tande ...[more]

PMID: 27689891

Similar Datasets

Project description:RationaleLiquid chromatography/photodiode array atmospheric pressure chemical ionization mass spectrometry (LC/PDA-APCI-MS) is used for the analysis of various carotenoid pigments in plants. Among them, it is difficult to distinguish between the isomeric violaxanthin/neoxanthin esters.MethodsThe yellow pigments of tomato petals were extracted with acetone, and the extracts were kept at -30°C to allow the contaminating triacylglycerols to settle out physically. The supernatants were analyzed using LC/PDA-APCI-MS with a high-resolution orbitrap mass spectrometer for their exact masses. The expected carotenoid esters were calculated with the combination of carotenoids and fatty acids, and they were matched with the experimental exact masses. The fatty acid structures in the carotenoid esters were also identified using collision-induced dissociation (CID) tandem mass spectrometry (MS/MS). The isomeric violaxanthin/neoxanthin esters were distinguished using CID MS/MS from their in-source dehydrated product ions as pseudoprecursor ions.ResultsThe in-source dehydrated ions [M - H2 O + H]+ of neoxanthin diesters predominated over their protonated molecules [M + H]+ in LC/MS. By contrast, the protonated molecules of violaxanthin diesters predominated. The 92 u loss product ions [M - H2 O - C7 H8 + H]+ were observed from the dehydrated violaxanthin diesters, but they were not generated from the dehydrated neoxanthin diesters in the CID MS/MS of their dehydrated pseudoprecursor ion [M - H2 O + H]+ .ConclusionsThe allene allyl carbocation in neoxanthin diesters was generated from dehydration after preferential protonation at the hydroxy group. The epoxide group of violaxanthin diesters opens easily after protonation; however, the dehydration did not proceed at this stage. The 92 u loss of C7 H8 was explained by an intramolecular [2 + 2] cycloaddition, which proceeded preferentially in dehydrated violaxanthin diesters because the carbocations in the dehydrated species were conjugated to the polyene and those double bonds were depolarized during CID MS/MS. Therefore, the isomeric neoxanthin/violaxanthin diesters were distinguished using LC/PDA-APCI-MS and MS/MS. This method was a practical and useful method of profiling the carotenoid esters of the yellow petals.

Project description:Castration resistant prostate cancer (CRPC), the fatal form of prostate cancer, remains androgen dependent despite castrate levels of circulating testosterone (T) and 5α-dihydrotestosterone (DHT). To investigate mechanisms by which the tumor can synthesize its own androgens and develop resistance to abiraterone acetate and enzalutamide, methods to measure a complete androgen profile are imperative. Here, we report the development and validation of a stable isotope dilution liquid chromatography electrospray ionization tandem mass spectrometric (SID-LC-ESI-MS/MS) method to quantify nine human hydroxy-androgens as picolinates, simultaneously with requisite specificity and sensitivity. In the established method, the fragmentation patterns of all nine hydroxy-androgen picolinates were identified, and [13C3]-5α-androstane-3α, 17β-diol and [13C3]-5α-androstane-3β, 17β-diol used as internal standards were synthesized enzymatically. Intra-day and inter-day precision and accuracy corresponds to the U.S. Food and Drug Administration Criteria for Bioanalytical Method Validation. The lower limit of quantitation (LLOQ) of nine hydroxy-androgens is 1.0pg to 2.5pg on column. Diols which have been infrequently measured: 5-androstene-3β, 17β-diol and 5α-androstane-3α, 17β-diol can be determined in serum at values as low as 1.0pg on column. The method also permits the quantitation of conjugated hydroxy-androgens following enzymatic digestion. While direct detection of steroid conjugates by electrospray-ionization tandem mass spectrometry has advantages the detection of unconjugated and conjugated steroids would require separate methods for each set of analytes. Our method was applied to pooled serum from male and female donors to provide reference values for both unconjugated and conjugated hydroxy-androgens. This method will allow us to interrogate the involvement of the conversion of 5-androstene-3β, 17β-diol to T, the backdoor pathway involving the conversion of 5α-androstane-3α, 17β-diol to DHT and the inactivation of DHT to 5α-androstane-3β, 17β-diol in advanced prostate cancer.

Dataset Information

Simultaneous Quantification of Antioxidant Compounds in Phellinus igniarius Using Ultra Performance Liquid Chromatography-Photodiode Array Detection-Electrospray Ionization Tandem Mass Spectrometry.

Publications

Simultaneous Quantification of Antioxidant Compounds in Phellinus igniarius Using Ultra Performance Liquid Chromatography-Photodiode Array Detection-Electrospray Ionization Tandem Mass Spectrometry.

Similar Datasets

OmicsDI is part of the ELIXIR infrastructure

Tweets