Karel Ventura

Comparison of pressurised fluid and ultrasonic extraction methods for analysis of plant antioxidants and their antioxidant capacity

The analytical method based on the high-performance liquid chromatography coupled with UV detection (HPLC/UV) for determination of selected antioxidants (i.e., esculetin, scopoletin, 7-hydroxycoumarine, rutin, xanthotoxin, 5-methoxypsoralen and quercetin) in plant material was developed. Pressurised fluid extraction (PFE) and ultrasonic extraction (USE) methods for the isolation of these compounds from ten real plant samples were used. Both extraction methods were optimised and compared to each other. For the proposed HPLC/UV method the LOQ values (limit of quantification) in the range from 22.7 (xanthotoxin) to 97.2 ng mL−1 (rutin) were obtained. For all extracts the antioxidant capacity based on the reduction of free 2,2-diphenyl-1-picrylhydrazyl radical (DPPH) was also determined. Results ranged from 82.04 to 94.43% of DPPH radical inhibition for PFE method and from 76.01 to 89.94% in the case of USE method.

Retention characteristics of some volatile compounds on Tenax GR

Abstract Breakthrough volumes (maximum sample volumes, Vmax.) of low-molecular-mass compounds on graphite-filled Tenax have been measured. Using Tenax GR the sampling volumes are greater than with Tenax GC or Tenax TA. Tenax GR can be used in environmental analysis for trapping and enriching traces of low-molecular-mass organic compounds.

Extraction of antioxidants from plants using ultrasonic methods and their antioxidant capacity

The analytical method based on the HPLC coupled with UV detection (HPLC-UV) for the determination of selected antioxidants (i.e. esculetin, scopoletin, 7-hydroxycoumarine, rutin, xanthotoxin, 5-methoxypsoralen and quercetin) in plant material was developed. Two ultrasonic extraction methods for the isolation of these compounds from the plants such as Mentha longifolia L., Mentha spicata L., Ruta graveolens L., Achyllea millefolium L., Plantago lanceolata L. and Coriandrum sativum L. were used. Both of these methods, i.e. ultrasonic probe and ultrasonic bath, were optimised and compared to each other. For the proposed HPLC-UV method LOQ values in the range from 22.7 (xanthotoxin) up to 97.2 ng/mL (rutin) were obtained. For all extracts the antioxidant capacity based on the reduction of free 2,2-diphenyl-1-picrylhydrazyl (DPPH) radical was also determined. Obtained results ranged from 10.11 up to 73.50% of DPPH radical inhibition.

Microextraction by packed sorbent (MEPS) as a suitable selective method for L-ascorbic acid determination in beverages

In this study the modern microextraction by packed sorbent (MEPS) method followed by HPLC-UV analysis was optimised and evaluated for determination of l-ascorbic acid (AA) content in beverages. In this case 300μL of sample was passed through silica BIN (barrel insert and needle assembly) and entrapped AA was eluted by 60μL of methanol-water (10%, v/v) solution. Recovery of the proposed method for three concentration levels ranged between 97.46% and 106.88% with relative standard deviation 8.7% (low conc.), 2.49% (medium conc.) and 1.98% (high). Obtained results of AA contents in real samples were in the ranges 56.5-195.4μg/mL and 130.4-1090.0μg/mL for ice-tea and fruit juice samples, respectively. Proposed method was compared with iodometric titration and DPPH methods, but microextraction method was found to be more selective for AA determination in tested samples.

Comparison of various techniques for the extraction and determination of antioxidants in plants.

The following extraction techniques have been used for extracting antioxidants (apigenin, coumarin, esculetin, umbelliferone, bergapten, quercetin, rutin, scopoletin and xanthotoxin) from plant material: supercritical fluid extraction, pressurized liquid extraction, extraction by means of Soxhlet apparatus, ultrasonic extraction in ultrasonic bath, and by means of ultrasonic probe. The analytical method based on HPLC-UV detection for the determination of selected antioxidants was developed. For all extracts the antioxidant capacity based on the reduction of free 2,2-diphenyl-1-picrylhydrazyl radical was also determined. Comparing all results the ultrasonic probe method using 0.75 g of sample extracted by 50 mL of acetonitrile in water (30%, v/v) for 25 min at room temperature and with amplitude at 60% (equal to 90 W) without pulsation was evaluated as the best tool. The most significant indicator demonstrating this statement is the antioxidant capacity expressed as gallic acid equivalent where the ultrasonic probe method showed the best results in 10 of 16 samples. Also the operability of ultrasonic probe extraction method compared to other tested methods is more favorable.

Headspace single‐drop microextraction of herbal essential oils

A method employing the headspace single-drop microextraction (HS-SDME) is presented for the determination of essential oils in dried herbal leaves. By optimising the key experimental parameters, a linear response for the individual target compounds was obtained in the concentration range from LOQ to 4 mg/mL (r(2) = 0.9912-0.9998), with LODs from 3.3 up to 20.5 microg per 100 g of dried leaves, and the repeatability within the RSD of 2.1-8.9%. The HS-SDME-based procedure, enabling a rapid and simple analysis of essential oils in herbs, was applied to selected real samples (nine essential oils in four different samples) in combination with GC-FID identification and quantification of the target volatiles.

Unremitting problems with chlorogenic acid Nomenclature: A review

Tento clanek shrnuje problematiku nazvoslovi isomerů patřicich do skupiny chlorogenových kyselin od jejich prvniho výskytu až dosud. Během desetileti bylo publikovano mnoho clanků zabývajicich se touto skupinou. Bohužel výzkumnici, kteři chtěli ziskat informace o tomto tematu, mohli být po přecteni několika clanků silně znechuceni. Kvůli postupným objevům a izolacim jednotlivých isomerů z nejrůznějsich matric a měnici se terminologii po těchto objevech jsou běžne nesrovnalosti mezi jednotlivými clanky. Přicinou těchto nesrovnalosti je hlavni sloucenina teto skupiny, a to 5-kafeoylchinova kyselina (znama jako kyselina chlorogenova) byla jako kyselina 3-kafeoylchinova opravdu nazývana před rokem 1976, kdy byla publikovana nova pravidla pro nazvoslovi. Nicmeně mnoho výzkumniků a take dodavatelů chemikalii zůstalo u použivani „pre UIPAC“ nazvoslovi a chybně nazývaji 3-kafeoylchinovou kyselinu jako kyselinu chlorogenovou, tj. hlavni substituent teto skupiny. Přestože několik praci s touto nesrovnalosti zapasi, tento problem stale přetrvava. Proto byla sepsana tato prace.

Supercritical fluid extraction of steroids from biological samples and first experience with solid-phase microextraction–liquid chromatography

Modern extraction techniques, supercritical fluid extraction (SFE) and solid-phase microextraction (SPME) were used for isolation of four corticosteroids from biological matrices. SFE was applied for extraction from solid matrices--hydromatrix and pig muscle. The effects of various extraction conditions were studied. Good recoveries of corticosteroids from hydromatrix were obtained under moderate extraction conditions and without modification of carbon dioxide. On the contrary, the best recoveries from spiked pig muscle were obtained with modified carbon dioxide. SPME was used for extraction from liquid samples--water and urine. The eventuality of the use of this fast solvent-free technique in steroid analysis is demonstrated. Several extraction conditions were optimized. Extracted steroids were analyzed by HPLC-UV and a special SPME-HPLC interface was used for combination with SPME.

Half-inhibition Concentrations of New Cholinesterase Inhibitors

The power of chosen carbamates and hydrazinium derivatives (carbazates) to inhibit the hydrolysis of acetylthiocholine by butyrylcholinesterase or acetylcholinesterase was tested. The determined pI50 values (= negative logarithm of the molar concentration inhibiting the enzyme activity by 50%) of the tested substances were compared with pI50 values of the commercially used drugs for the Alzheimer’s disease treatment - rivastigmine and galanthamine.

Comparison of supercritical fluid and Soxhlet extractions for the isolation of nitro compounds from soils

Supercritical fluid extraction (SFE) with CO(2), a clean and rapid alternative to conventional Soxhlet extraction, was investigated for the extraction of nitro compounds from soil samples. Quantitative extraction by SFE was accomplished at a pressure of 25 MPa and an extraction temperature of 60 degrees C, for 30 min in dynamic mode and using acetonitrile as modifier, and the results were comparable with those obtained by acetonitrile Soxhlet extraction (3 h) for all soil samples. Extracts from these two procedures were analyzed by gas chromatography coupled with mass spectrometry. Quantitative reproducibility for SFE extracts was acceptable (RSD 2-10%), and the quantity of solvent was reduced from 160 mL for Soxhlet extraction to 5 mL in the case of SFE.