LC-MS Method for the Detection and Quantification of Ursolic Acid and Uvaol Levels in Olive Leaves and Oregano

Author(s):  
Naser F. Al-Tannak ◽  
Ladislav Novotny

Ursolic acid and uvaol belong to pentacyclic triterpenes are both secondary metabolites with significant biological activity. Ursolic acid and uvaol are exist in many natural matrices such as olive leaves, oregano and thymus. Therefore, a new rapid and validated UPLC method was developed to identify and quantify ursolic acid and uvaol in dry olive leaves (Olea europaea L.) planted in Kuwait and dry oregano (Origanum vulgare L.) planted in Palestine and Spain. The separation of ursolic acid and uvaol was achieved by using BEH Phenyl (1.7 μm, 2.1 x 100 mm) analytical column (Waters® Acquity UPLC) and a mobile phase composed of water and acetonitrile (37:63 v/v). Solid-phase extraction cartridges (HyperSep™) was used to extract ursolic acid and uvaol from natural matrices. Ursolic acid and uvaol were detected in all-natural matrices used. The concentrations of ursolic acid and uvaol in olive leaves were 55.10 μg/g ± 0.72 and 314.29 μg/g ± 0.97, respectively. In contrast, ursolic acid and uvaol concentrations in oregano brands were ranging from 25.57 μg/g ± 0.35- 28.70 μg/g ± 0.36 and 19.07 μg/g ± 0.38 - 48.10 μg/g ± 0.62, respectively. In conclusion, the developed method was capable to identify and determine ursolic acid and uvaol in pure powder and natural matrices with good linearity, accuracy and precision.

2005 ◽  
Vol 51 ◽  
pp. 23-28 ◽  
Author(s):  
Violeta Ivanova ◽  
Dragica Zendelovska ◽  
Marina Stefova

A simple, rapid and precise HPLC method has been developed for the assay of hydrochlorothiazide in urine. The clean-up of the urine samples was carried out by solid-phase extraction using HLB cartridges. Extraction recovery was 94.00-100.28 %. HPLC separation was performed with isocratic elution on Hypersil BDS C18 column (100 x 4.0 mm I.D., 3 µm particle size) protected with appropriate guard column. The mobile phase was 18 % acetonitrile and 0.025 mol/L solution of KH2PO4, pH 4 at flow rate of 0.3 mL/min. Detection of the substances was performed at 220 nm. The calibration curves were linear in the range of 2-50 µg/mL. The developed method is validated by checking its accuracy, precision and stability. The detection limit is 2 µg/mL hydrochlorothiazide. The method is proved to be convenient for routine analysis of hydrochlorothiazide in urine.


1996 ◽  
Vol 79 (3) ◽  
pp. 645-651 ◽  
Author(s):  
Christiaan A J Hajee ◽  
Nel Haagsma

Abstract An analytical method is presented for liquid chromatographic (LC) determination of mebendazole (MBZ), hydroxymebendazole (MBZ-OH), and aminomebendazole (MBZ-NH2) in eel muscle tissue. Muscle tissue is extracted with ethyl acetate at pH 7.5. After addition of n-hexane, the extract is cleaned up and concentrated on an aminopropyl solid-phase extraction column. The test solutions are analyzed isocratically on a ChromSpher B LC column with acetonitrile–phosphate buffer, pH 6.2, as mobile phase. Limits of detection and quantitation were 0.7 and 1.1 ¼g/kg, respectively, for MBZOH; 1.4 and 2.3 ¼g/kg, respectively, for MBZ; and 1.5 and 2.1 ¼g/kg, respectively, for MBZ-NH2. Interand intraday coefficients of variation were 3.5 and 3.4%, respectively, for MBZ-OH; 2.5 and 3.1%, respectively, for MBZ; and 5.8 and 4.8%, respectively, for MBZ-NH2. Mean recoveries were 90% for MBZ, 74% for MBZ-NH2, and 92% for MBZ-OH. A linear range of applicability of at least 10–1000 ¼g/kg was found for each analyte. Incurred MBZ-NH2 (181.3 ¼g/kg) was identified in eel muscle tissue apart from MBZ (23.7 ¼g/kg) after 48 h exposure ina treatment bath containing MBZ at 1 mg/L.


2012 ◽  
Vol 2012 ◽  
pp. 1-5
Author(s):  
Alex S. M. S. J. Santos ◽  
Adriano Aquino ◽  
Luciane P. C. Romão ◽  
Sandro Navickiene

Natural peat was tested for extraction of pyrimethanil, flumetralin, and krexosim-methyl from water, with analysis using gas chromatography-mass spectrometry (GC-MS) in selected ion monitoring mode (SIM). Experiments were carried out at one fortification level (0.1 μg L−1) and resulted in recoveries in the range 41–96%, with RSD values between 6.8 and 12.6% for natural peat as sorbent. Detection and quantification limits ranged from 0.02 to 0.05 μg L−1 and from 0.07 to 0.1 μg L−1, respectively, for the different pesticides studied. The method developed was linear over the range tested (0.07–4.0 μg L−1), with correlation coefficients ranging from 0.9919 to 0.9989. Comparison between peat and commercial sorbents (C18-bonded silica, ENVI-Carb, Florisil, silica gel, ENVI-Carb/LC-NH2) showed better performance of peat sorbent for flumetralin and kresoxim-methyl.


2020 ◽  
Vol 12 (5) ◽  
pp. 638-645
Author(s):  
Huan Yu ◽  
Haiyan Liu ◽  
Chunliu Yang ◽  
Xiaoya Pang ◽  
Miaomiao Zhang ◽  
...  

A hybrid monolith was prepared and used as a sorbent for online enrichment and purification of ursolic acid from medicinal plants.


2008 ◽  
Vol 31 (20) ◽  
pp. 3573-3580 ◽  
Author(s):  
Hanmao Liu ◽  
Chunhai Liu ◽  
Xiaojing Yang ◽  
Songjun Zeng ◽  
Yuanqin Xiong ◽  
...  

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