Fractionation of Labisia Pumila using Solid-Phase Extraction for Extraction of Gallic Acid

2014 ◽  
Vol 69 (4) ◽  
Author(s):  
Siti Nadiah Mohd Abdah ◽  
Mohammad Roji Sarmidi ◽  
Harisun Yaakob ◽  
Ismail Ware
Keyword(s):  
Solid Phase Extraction ◽  
Gallic Acid ◽  
Solid Phase ◽  
Water Extract ◽  
Reversed Phase ◽  
Extraction Column ◽  
Solvent Mixtures ◽  
Phase Extraction ◽  
Water Solvent ◽  
Labisia Pumila

Phenolics are the most ample secondary metabolites of plants and have drawn increasing attention in their applications in health supplement and functional cosmetic. This is due to their strong antioxidant properties and their marked effects in the inhibition of several oxidative stress associated metabolic disorder such as cancer and aging. In Labisia pumila, gallic acid (3,4,5-Trihydroxybenzoic acid) was found to be one of the most abundant secondary metabolite. It has been proposed as a biomarker in cosmetic and food supplement applications. In this research the identification and isolation of gallic acid were carried out. Different sorbent of solid-phase extraction (SPE) column were used for the fractionation of Labisia pumila var Alata water extract and the amount of gallic acid present in the fractions were quantified. The aim is to identify the better sorbent-solvent combination in SPE that result in higher recovery of gallic acid from Labisia pumila var Alata water extract. A range of solvent mixtures of 20%, 40%, 60% and 80% methanol (Me Oh)-water was used. Gallic acid was successfully extracted and identified from Labisia pumila. From this discovery, C18 silica reversed phase solid phase extraction column could extracts highest gallic acid from Labisia pumila var Alata water extract. Retention of analyte from  the sample from second elution using 80% methanol-water Solvent may be used as the best method to extract the compound from Labisia Pumila var Alata since it has been reported to have various bioactivities such as high antioxidant activity and cytotoxic against many diseases. Using C18 silica reversed phase in SPE as a fractionation and extraction of gallic acid from Labisia pumila var Alata can be achieved for application purpose or future studies.

scholarly journals Determination of urinary free cortisol by HPLC

1997 ◽  
Vol 43 (8) ◽  
pp. 1386-1391 ◽  
Author(s):  
Ursula Turpeinen ◽  
Helene Markkanen ◽  
Matti Välimäki ◽  
Ulf-Håkan Stenman
Keyword(s):  
Solid Phase Extraction ◽  
Mobile Phase ◽  
Solid Phase ◽  
Internal Standard ◽  
Reversed Phase ◽  
Hplc Method ◽  
Extraction Column ◽  
Phase Extraction ◽  
Free Cortisol

Abstract We here report a reversed-phase HPLC method for the determination of free cortisol in human urine, using methylprednisolone as the internal standard. Before chromatography, samples were extracted with a C18 solid-phase extraction column and the steroids were separated on a LiChrospher 100 C18 column with a mobile phase of methanol/acetonitrile/water (43/3/54 by vol). Linearity, precision, and accuracy of the method were established. The detection limit was 10 pmol of cortisol, and total CVs were <8%. With various solid-phase extraction columns the recovery of cortisol was 36–97%; recovery of the internal standard was 43–85%. Study of interference by 6 other steroids and metabolites and 24 drugs showed that carbamazepine and digoxin partly overlapped with cortisol, but this interference could be reduced by modification of the mobile phase. The HPLC method was compared with an RIA and an automated immunoassay method. The results obtained by HPLC averaged 40% of the RIA values.

scholarly journals An Efficient Solid-Phase Extraction-Based Liquid Chromatography Method to Simultaneously Determine Diastereomers α-Tocopherol, Other Tocols, and Retinol Isomers in Infant Formula

2021 ◽  
Vol 2021 ◽  
pp. 1-8
Author(s):  
Baifen Huang ◽  
Zengxuan Cai ◽  
Jingshun Zhang ◽  
Jiaojiao Xu
Keyword(s):  
Liquid Chromatography ◽  
Solid Phase Extraction ◽  
Infant Formula ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Reversed Phase ◽  
Extraction Column ◽  
Phase Extraction ◽  
Chromatography Method ◽  
Macroporous Silica

The separation and simultaneous quantitation of diastereomers of DL-α-tocopherol, eight tocol forms, and retinols (trans and cis) have been conducted by reversed-phase liquid chromatography followed by solid-phase extraction. A chiral silica stationary phase modified with polysaccharide derivative on the monodisperse macroporous silica gel (Unichiral OD-5H column, 150 mm × 4.6 mm, 5 μm, NanoMicro Technology Co., Ltd.) was employed for eluting each target compound. Instead of conventional solvent extract, a green and eco-friendly solid-phase extraction column, packing with nonpolar polystyrene divinylbenzene, was optimized in terms of capacity and solvent used in steps. Validation of the method was examined and confirmed to be satisfactory, with excellent linearity regression (r > 0.9999), acceptable accuracy (74.66%∼112.92%), and precision (0.20%∼10.52%) results. Limit of detection ranged from 0.05 mg·kg−1 (retinols) to 0.4 mg·kg−1 (tocols). The method was checked by infant formula reference material SRM 1849a as well, which illustrated good agreement of mass fraction with certified value and enriched the important isomer data.

scholarly journals Determination of Antiviral Drugs and Their Metabolites Using Micro-Solid Phase Extraction and UHPLC-MS/MS in Reversed-Phase and Hydrophilic Interaction Chromatography Modes

Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2123
Author(s):  
Luboš Fical ◽  
Maria Khalikova ◽  
Hana Kočová Vlčková ◽  
Ivona Lhotská ◽  
Zuzana Hadysová ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Liquid Chromatography ◽  
Tandem Mass Spectrometry ◽  
Solid Phase Extraction ◽  
Solid Phase ◽  
Gradient Elution ◽  
Reversed Phase ◽  
Tandem Mass ◽  
Phase Extraction ◽  
Hydrophilic Interaction

Two new ultra-high performance liquid chromatography (UHPLC) methods for analyzing 21 selected antivirals and their metabolites were optimized, including sample preparation step, LC separation conditions, and tandem mass spectrometry detection. Micro-solid phase extraction in pipette tips was used to extract antivirals from the biological material of Hanks balanced salt medium of pH 7.4 and 6.5. These media were used in experiments to evaluate the membrane transport of antiviral drugs. Challenging diversity of physicochemical properties was overcome using combined sorbent composed of C18 and ion exchange moiety, which finally allowed to cover the whole range of tested antivirals. For separation, reversed-phase (RP) chromatography and hydrophilic interaction liquid chromatography (HILIC), were optimized using extensive screening of stationary and mobile phase combinations. Optimized RP-UHPLC separation was carried out using BEH Shield RP18 stationary phase and gradient elution with 25 mmol/L formic acid in acetonitrile and in water. HILIC separation was accomplished with a Cortecs HILIC column and gradient elution with 25 mmol/L ammonium formate pH 3 and acetonitrile. Tandem mass spectrometry (MS/MS) conditions were optimized in both chromatographic modes, but obtained results revealed only a little difference in parameters of capillary voltage and cone voltage. While RP-UHPLC-MS/MS exhibited superior separation selectivity, HILIC-UHPLC-MS/MS has shown substantially higher sensitivity of two orders of magnitude for many compounds. Method validation results indicated that HILIC mode was more suitable for multianalyte methods. Despite better separation selectivity achieved in RP-UHPLC-MS/MS, the matrix effects were noticed while using both chromatographic modes leading to signal enhancement in RP and signal suppression in HILIC.

Development of a solid-phase extraction – spectrofluorimetric method for trace glutathione determination

2011 ◽  
Vol 89 (4) ◽  
pp. 517-523 ◽  
Author(s):  
Ke-Jing Huang ◽  
Cong-Hui Han ◽  
Ying-Ying Wu ◽  
Chao-Qun Han ◽  
De-Jun Niu ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Limit Of Detection ◽  
Solid Phase ◽  
Signal To Noise Ratio ◽  
Calibration Graph ◽  
Extraction Column ◽  
Phase Extraction ◽  
Selective Reaction ◽  
Spectrofluorimetric Method ◽  
Relative Standard

A simple and efficient solid-phase extraction – spectrofluorimetric method has been developed to determine glutathione (GSH). Fluorescent probe N-(4,4-difluoro-5,7-dimethyl-4-bora-3a,4a-diaza-s-indacene-3-yl)methyl)iodoacetamide (BODIPY Fl-C1-IA) was used as the derivatization reagent. The procedure was based on a BODIPY Fl-C1-IA selective reaction with GSH to form the highly fluorescent product BODIPY Fl-C1-IA–GSH, using a solid-phase extraction column and spectrofluorimetric determination. The variables affecting analytical performance were studied and optimized. The calibration graph using the preconcentration system for GSH was linear over the range of 1–200 nmol/L with a limit of detection of 0.05 nmol/L (signal-to-noise ratio = 3). The relative standard deviation for six replicate determinations of GSH at the 100 nmol/L concentration level was 3.9%. The method was applied to water samples and average recoveries between 87.5% and 111.5% were obtained for spiked samples.

Rapid and simple determination of nicorandil in rat plasma using a solid-phase extraction column

1990 ◽  
Vol 528 ◽  
pp. 509-516 ◽  
Author(s):  
Yutaka Gomita ◽  
Katsushi Furuno ◽  
Kohei Eto ◽  
Tamotsu Fukuda ◽  
Yasunori Araki ◽  
...  
Keyword(s):  
Solid Phase Extraction ◽  
Solid Phase ◽  
Rat Plasma ◽  
Extraction Column ◽  
Phase Extraction ◽  
Solid Phase Extraction Column
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