A UHPLC method for the rapid separation and quantification of phytosterols using tandem UV/Charged aerosol detection - A comparison of both detection techniques

Kód výsledku v IS VaVaI

<a href="https://www.isvavai.cz/riv?ss=detail&h=RIV%2F00216208%3A11160%2F17%3A10362174" target="_blank" >RIV/00216208:11160/17:10362174 - isvavai.cz</a>

Výsledek na webu

<a href="http://www.sciencedirect.com/science/article/pii/S0731708517305216" target="_blank" >http://www.sciencedirect.com/science/article/pii/S0731708517305216</a>

DOI - Digital Object Identifier

<a href="http://dx.doi.org/10.1016/j.jpba.2017.03.057" target="_blank" >10.1016/j.jpba.2017.03.057</a>

Jazyk výsledku

angličtina

Název v původním jazyce

A UHPLC method for the rapid separation and quantification of phytosterols using tandem UV/Charged aerosol detection - A comparison of both detection techniques

Popis výsledku v původním jazyce

The presented work describes the development and validation of a rapid UHPLC-UV/CAD method using a core-shell particle column for the separation and quantitative analysis of seven plant sterols and stanols. The phytosterols (ergosterol, brassicasterol, campesterol, fucosterol, stigmasterol, and beta-sitosterol) and the phytostanol stigmastanol were separated and analyzed in 8.5 min. The sample pre-treatment procedure was optimized to be less time-consuming than any other published method, especially due to no need of derivatization, evaporation and even reconstitution step. The chromatographic separation was performed on the Kinetex 1.7 mu Phenyl-hexyl column (100 x 2.1 mm) with a mobile phase acetoni-trile/water according to the gradient program at a flow rate of 0.9 mL min(-1) and a temperature of 60 degrees C. A tandem connection of PDA and CAD (Corona Charged Aerosol Detector) was used and both detection techniques were compared. The method was validated using saponification as a first step in sample pretreatment and an universal CAD as the detector. Recoveries for all analyzed compounds were between 95.4% and 103.4% and relative standard deviation ranged from 1.0% to 5.8% for within-day and from 1.4% to 6.7% for between-day repeatability. The limits of detection were in the range of 0.4-0.6 mu g mL(-1) for standard solutions and 0.3-1.2 mu g mL(-1) for phytosterols in real samples. Although several gradient programs and different stationary phases were tested, two compounds, campesterol and campestanol, were not separated. Their peak was quantified as a sum of both analytes.

Název v anglickém jazyce

A UHPLC method for the rapid separation and quantification of phytosterols using tandem UV/Charged aerosol detection - A comparison of both detection techniques

Popis výsledku anglicky

The presented work describes the development and validation of a rapid UHPLC-UV/CAD method using a core-shell particle column for the separation and quantitative analysis of seven plant sterols and stanols. The phytosterols (ergosterol, brassicasterol, campesterol, fucosterol, stigmasterol, and beta-sitosterol) and the phytostanol stigmastanol were separated and analyzed in 8.5 min. The sample pre-treatment procedure was optimized to be less time-consuming than any other published method, especially due to no need of derivatization, evaporation and even reconstitution step. The chromatographic separation was performed on the Kinetex 1.7 mu Phenyl-hexyl column (100 x 2.1 mm) with a mobile phase acetoni-trile/water according to the gradient program at a flow rate of 0.9 mL min(-1) and a temperature of 60 degrees C. A tandem connection of PDA and CAD (Corona Charged Aerosol Detector) was used and both detection techniques were compared. The method was validated using saponification as a first step in sample pretreatment and an universal CAD as the detector. Recoveries for all analyzed compounds were between 95.4% and 103.4% and relative standard deviation ranged from 1.0% to 5.8% for within-day and from 1.4% to 6.7% for between-day repeatability. The limits of detection were in the range of 0.4-0.6 mu g mL(-1) for standard solutions and 0.3-1.2 mu g mL(-1) for phytosterols in real samples. Although several gradient programs and different stationary phases were tested, two compounds, campesterol and campestanol, were not separated. Their peak was quantified as a sum of both analytes.

Druh

J_imp - Článek v periodiku v databázi Web of Science

CEP obor

—

OECD FORD obor

30104 - Pharmacology and pharmacy

Projekt

—

Návaznosti

S - Specificky vyzkum na vysokych skolach<br>I - Institucionalni podpora na dlouhodoby koncepcni rozvoj vyzkumne organizace

Rok uplatnění

2017

Kód důvěrnosti údajů

S - Úplné a pravdivé údaje o projektu nepodléhají ochraně podle zvláštních právních předpisů

Název periodika

Journal of Pharmaceutical and Biomedical Analysis

ISSN

0731-7085

e-ISSN

—

Svazek periodika

140

Číslo periodika v rámci svazku

June

Stát vydavatele periodika

GB - Spojené království Velké Británie a Severního Irska

Počet stran výsledku

7

Strana od-do

274-280

Kód UT WoS článku

000402850500033

EID výsledku v databázi Scopus

2-s2.0-85016828304