Validated Method for the Characterization and Quantification of Extractable and Nonextractable Ellagitannins after Acid Hydrolysis in Pomegranate Fruits, Juices, and Extracts.

PubMed

García-Villalba, Rocío; Espín, Juan Carlos; Aaby, Kjersti; Alasalvar, Cesarettin; Heinonen, Marina; Jacobs, Griet; Voorspoels, Stefan; Koivumäki, Tuuli; Kroon, Paul A; Pelvan, Ebru; Saha, Shikha; Tomás-Barberán, Francisco A

2015-07-29

Pomegranates are one of the main highly valuable sources of ellagitannins. Despite the potential health benefits of these compounds, reliable data on their content in pomegranates and derived extracts and food products is lacking, as it is usually underestimated due to their complexity, diversity, and lack of commercially available standards. This study describes a new method for the analysis of the extractable and nonextractable ellagitannins based on the quantification of the acid hydrolysis products that include ellagic acid, gallic acid, sanguisorbic acid dilactone, valoneic acid dilactone, and gallagic acid dilactone in pomegranate samples. The study also shows the occurrence of ellagitannin C-glycosides in pomegranates. The method was optimized using a pomegranate peel extract. To quantify nonextractable ellagitannins, freeze-dried pomegranate fruit samples were directly hydrolyzed with 4 M HCl in water at 90 °C for 24 h followed by extraction of the pellet with dimethyl sulfoxide/methanol (50:50, v/v). The method was validated and reproducibility was assessed by means of an interlaboratory trial, showing high reproducibility across six laboratories with relative standard deviations below 15%. Their applicability was demonstrated in several pomegranate extracts, different parts of pomegranate fruit (husk, peels, and mesocarp), and commercial juices. A large variability has been found in the ellagitannin content (150-750 mg of hydrolysis products/g) and type (gallagic acid/ellagic acid ratios between 4 and 0.15) of the 11 pomegranate extracts studied.

Comparison of four extraction/methylation analytical methods to measure fatty acid composition by gas chromatography in meat.

PubMed

Juárez, M; Polvillo, O; Contò, M; Ficco, A; Ballico, S; Failla, S

2008-05-09

Four different extraction-derivatization methods commonly used for fatty acid analysis in meat (in situ or one-step method, saponification method, classic method and a combination of classic extraction and saponification derivatization) were tested. The in situ method had low recovery and variation. The saponification method showed the best balance between recovery, precision, repeatability and reproducibility. The classic method had high recovery and acceptable variation values, except for the polyunsaturated fatty acids, showing higher variation than the former methods. The combination of extraction and methylation steps had great recovery values, but the precision, repeatability and reproducibility were not acceptable. Therefore the saponification method would be more convenient for polyunsaturated fatty acid analysis, whereas the in situ method would be an alternative for fast analysis. However the classic method would be the method of choice for the determination of the different lipid classes.

Analysis of Phenolic Compounds and Antioxidant Activity in Wild Blackberry Fruits

PubMed Central

Oszmiański, Jan; Nowicka, Paulina; Teleszko, Mirosława; Wojdyło, Aneta; Cebulak, Tomasz; Oklejewicz, Krzysztof

2015-01-01

Twenty three different wild blackberry fruit samples were assessed regarding their phenolic profiles and contents (by LC/MS quadrupole time-of-flight (QTOF) and antioxidant activity (ferric reducing ability of plasma (FRAP) and 2,2-azinobis (3-ethyl-benzothiazoline-6-sulfonic acid) (ABTS)) by two different extraction methods. Thirty four phenolic compounds were detected (8 anthocyanins, 15 flavonols, 3 hydroxycinnamic acids, 6 ellagic acid derivatives and 2 flavones). In samples, where pressurized liquid extraction (PLE) was used for extraction, a greater increase in yields of phenolic compounds was observed, especially in ellagic acid derivatives (max. 59%), flavonols (max. 44%) and anthocyanins (max. 29%), than after extraction by the ultrasonic technique extraction (UAE) method. The content of phenolic compounds was significantly correlated with the antioxidant activity of the analyzed samples. Principal component analysis (PCA) revealed that the PLE method was more suitable for the quantitative extraction of flavonols, while the UAE method was for hydroxycinnamic acids. PMID:26132562

Optimization of acidic extraction of astaxanthin from Phaffia rhodozyma *

PubMed Central

Ni, Hui; Chen, Qi-he; He, Guo-qing; Wu, Guang-bin; Yang, Yuan-fan

2008-01-01

Optimization of a process for extracting astaxanthin from Phaffia rhodozyma by acidic method was investigated, regarding several extraction factors such as acids, organic solvents, temperature and time. Fractional factorial design, central composite design and response surface methodology were used to derive a statistically optimal model, which corresponded to the following optimal condition: concentration of lactic acid at 5.55 mol/L, ratio of ethanol to yeast dry weight at 20.25 ml/g, temperature for cell-disruption at 30 °C, and extraction time for 3 min. Under this condition, astaxanthin and the total carotenoids could be extracted in amounts of 1294.7 μg/g and 1516.0 μg/g, respectively. This acidic method has advantages such as high extraction efficiency, low chemical toxicity and no special requirement of instruments. Therefore, it might be a more feasible and practical method for industrial practice. PMID:18196613

Solvent extraction system for plutonium colloids and other oxide nano-particles

DOEpatents

Soderholm, Lynda; Wilson, Richard E; Chiarizia, Renato; Skanthakumar, Suntharalingam

2014-06-03

The invention provides a method for extracting plutonium from spent nuclear fuel, the method comprising supplying plutonium in a first aqueous phase; contacting the plutonium aqueous phase with a mixture of a dielectric and a moiety having a first acidity so as to allow the plutonium to substantially extract into the mixture; and contacting the extracted plutonium with second a aqueous phase, wherein the second aqueous phase has a second acidity higher than the first acidity, so as to allow the extracted plutonium to extract into the second aqueous phase. The invented method facilitates isolation of plutonium polymer without the formation of crud or unwanted emulsions.

Fast and comprehensive analysis of secondary metabolites in cocoa products using ultra high-performance liquid chromatography directly after pressurized liquid extraction.

PubMed

Damm, Irina; Enger, Eileen; Chrubasik-Hausmann, Sigrun; Schieber, Andreas; Zimmermann, Benno F

2016-08-01

Fast methods for the extraction and analysis of various secondary metabolites from cocoa products were developed and optimized regarding speed and separation efficiency. Extraction by pressurized liquid extraction is automated and the extracts are analyzed by rapid reversed-phase ultra high-performance liquid chromatography and normal-phase high-performance liquid chromatography methods. After extraction, no further sample treatment is required before chromatographic analysis. The analytes comprise monomeric and oligomeric flavanols, flavonols, methylxanthins, N-phenylpropenoyl amino acids, and phenolic acids. Polyphenols and N-phenylpropenoyl amino acids are separated in a single run of 33 min, procyanidins are analyzed by normal-phase high-performance liquid chromatography within 16 min, and methylxanthins require only 6 min total run time. A fourth method is suitable for phenolic acids, but only protocatechuic acid was found in relevant quantities. The optimized methods were validated and applied to 27 dark chocolates, one milk chocolate, two cocoa powders and two food supplements based on cocoa extract. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Choice of solvent extraction technique affects fatty acid composition of pistachio (Pistacia vera L.) oil.

PubMed

Abdolshahi, Anna; Majd, Mojtaba Heydari; Rad, Javad Sharifi; Taheri, Mehrdad; Shabani, Aliakbar; Teixeira da Silva, Jaime A

2015-04-01

Pistachio (Pistacia vera L.) oil has important nutritional and therapeutic properties because of its high concentration of essential fatty acids. The extraction method used to obtain natural compounds from raw material is critical for product quality, in particular to protect nutritional value. This study compared the fatty acid composition of pistachio oil extracted by two conventional procedures, Soxhlet extraction and maceration, analyzed by a gas chromatography-flame ionization detector (GC-FID). Four solvents with different polarities were tested: n-hexane (Hx), dichloromethane (DCM), ethyl acetate (EtAc) and ethanol (EtOH). The highest unsaturated fatty acid content (88.493 %) was obtained by Soxhlet extraction with EtAc. The Soxhlet method extracted the most oleic and linolenic acids (51.99 % and 0.385 %, respectively) although a higher concentration (36.32 %) of linoleic acid was extracted by maceration.

Microbial process for the preparation of acetic acid, as well as solvent for its extraction from the fermentation broth

DOEpatents

Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

2007-03-27

A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. Solvent mixtures formed of such a modified solvent with a desired co-solvent, preferably a low boiling hydrocarbon, are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

Microbial process for the preparation of acetic acid, as well as solvent for its extraction from the fermentation broth

DOEpatents

Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

2004-06-22

A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. Solvent mixtures formed of such a modified solvent with a desired co-solvent, preferably a low boiling hydrocarbon, are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

Determination of fatty acid composition and quality characteristics of oils from palm fruits using solvent extraction

NASA Astrophysics Data System (ADS)

Kasmin, Hasimah; Lazim, Azwan Mat; Awang, Roila

2015-09-01

Palm oil contains about 45% of saturated palmitic acid and 39% of mono-unsaturated oleic acid. Investigations made in the past to trace the fatty acid composition in palm revealed that ripeness of fresh fruit bunch (FFB) affect oil composition. However, there is no evidence that processing operations affect oil composition, although different stage of processing does affect the quality of oil extracted. An improved method for sterilizing the oil palm fruits by dry heating, followed by oil extraction has been studied. This method eliminates the use of water, thus, increasing the extraction of lipid soluble. The objective of this study is to determine the possibility production of palm oil with different fatty acid composition (FAC) as well as the changes in quality from conventional milling. The unripe and ripe FFB were collected, sterilized and extracted using different method of solvent extraction. Preliminary data have shown that variation in FAC will also alter the physical and chemical properties of the oil extracted.

Determination of betulinic acid, oleanolic acid and ursolic acid from Achyranthes aspera L. using RP-UFLC-DAD analysis and evaluation of various parameters for their optimum yield.

PubMed

Pai, Sandeep R; Upadhya, Vinayak; Hegde, Harsha V; Joshi, Rajesh K; Kholkute, Sanjiva D

2016-03-01

Achyranthes aspera L. is a well known herb commonly used in traditional system of Indian medicine to treat various disorders, such as cough, dysentery, gonorrhea, piles, kidney stone, pneumonia, renal dropsy, skin eruptions, snake bite, etc. Here, we used RP-UFLC-DAD method for determining triterpenoids betulinic acid (BA), oleanolic acid (OA) and ursolic acid (UA) from A. aspera. Optimum yield of these compounds were studied and evaluated using parameters viz., method of extraction, time of extraction, age of plant and plant parts (leaves, stem and roots). Linear relationships in RP-UFLC-DAD analysis were obtained in the range 0.05-100 µg/mL with 0.035, 0.042 and 0.033 µg/mL LOD for BA, OA and UA, respectively. Of the variables tested, extraction method and parts used significantly affected content yield. Continuous shaking extraction (CSE) at ambient temperature gave better extraction efficiency than exposure to ultra sonic extraction (USE) or microwave assisted extraction (MAE) methods. The highest content of BA, OA and UA were determined individually in leaf, stem and root extracts with CSE. Collective yield of these triterpenoids were higher in leaf part exposed to 15 min USE method. To best of our knowledge, the study newly reports UA from A. aspera and the same was confirmed using ATR-FT-IR studies. This study explains the distribution pattern of these major triterpenoids and optimum extraction parameters in detail.

Effects of ultrahigh pressure extraction on yield and antioxidant activity of chlorogenic acid and cynaroside extracted from flower buds of Lonicera japonica.

PubMed

Hu, Wen; Guo, Ting; Jiang, Wen-Jun; Dong, Guang-Li; Chen, Da-Wei; Yang, Shi-Lin; Li, He-Ran

2015-06-01

The present study was designed to establish and optimize a new method for extracting chlorogenic acid and cynaroside from Lonicera japonica Thunb. through orthogonal experimental designl. A new ultrahigh pressure extraction (UPE) technology was applied to extract chlorogenic acid and cynaroside from L. japonica. The influential factors, including solvent type, ethanol concentration, extraction pressure, time, and temperature, and the solid/liquid ratio, have been studied to optimize the extraction process. The optimal conditions for the UPE were developed by quantitative analysis of the extraction products by HPLC-DAD in comparison with standard samples. In addition, the microstructures of the medicinal materials before and after extraction were studied by scanning electron microscopy (SEM). Furthermore, the extraction efficiency of different extraction methods and the 2, 2-diphenyl-1-picrylhydrazyl (DPPH) radical scavenging activities of the extracts were investigated. The optimal conditions for extracting chlorogenic acid and cynaroside were as follows: ethanol concentration, 60%; extraction pressure, 400 MPa; extraction time, 2 min; extraction temperature, 30 °C; and the solid/liquid ratio, 1 : 50. Under these conditions, the yields of chlorogenic acid and cynaroside were raised to 4.863% and 0.080%, respectively. Compared with other extraction methods, such as heat reflux extraction (HRE), ultrasonic extraction (UE), and Sohxlet extraction (SE), the UPE method showed several advantages, including higher extraction yield, shorter extraction time, lower energy consumption, and higher purity of the extracts. This study could help better utilize L. japonica flower buds as a readily accessible source of natural antioxidants in food and pharmaceutical industries. Copyright © 2015 China Pharmaceutical University. Published by Elsevier B.V. All rights reserved.

Rare Earth Extraction from NdFeB Magnet Using a Closed-Loop Acid Process.

PubMed

Kitagawa, Jiro; Uemura, Ryohei

2017-08-14

There is considerable interest in extraction of rare earth elements from NdFeB magnets to enable recycling of these elements. In practical extraction methods using wet processes, the acid waste solution discharge is a problem that must be resolved to reduce the environmental impact of the process. Here, we present an encouraging demonstration of rare earth element extraction from a NdFeB magnet using a closed-loop hydrochloric acid (HCl)-based process. The extraction method is based on corrosion of the magnet in a pretreatment stage and a subsequent ionic liquid technique for Fe extraction from the HCl solution. The rare earth elements are then precipitated using oxalic acid. Triple extraction has been conducted and the recovery ratio of the rare earth elements from the solution is approximately 50% for each extraction process, as compared to almost 100% recovery when using a one-shot extraction process without the ionic liquid but with sufficient oxalic acid. Despite its reduced extraction efficiency, the proposed method with its small number of procedures at almost room temperature is still highly advantageous in terms of both cost and environmental friendliness. This study represents an initial step towards realization of a closed-loop acid process for recycling of rare earth elements.

A comparison of juice extraction methods in the pungency measurement of onion bulbs.

PubMed

Yoo, Kil Sun; Lee, Eun Jin; Hamilton, Brian K; Patil, Bhimanagouda S

2016-02-01

Onion pungency is estimated by measuring the pyruvic acid content in juice extracted from fresh tissues. We compared pyruvic acid content and its variation in the juices extracted by the pressing, maceration, blending with no water, or blending with water (blend/water) methods. There were considerable differences in the pyruvic acid content and coefficient of variation (CV) among these methods, and there was an interaction between the onion cultivars and the juice extraction methods. The pressing method showed over 30% CV in the quartered or composite samples. The blend/water method showed the greatest pyruvic acid content in the shortday-type ('TG1015Y' and 'Texas Early White') onions, while the pressing method showed the greatest pyruvic acid content in the longday-type onions. The blend/water method, which gave ratios between 1:1 and 1:4 (w/w), showed the same pyruvic acid content. The blending (no water) method had the highest correlation, followed by the maceration method. The lowest correlations were found with the pressing method and the blend/water method. Complete homogenisation of tissues with 1:1 or greater ratios of water was necessary for the maximum consistency and full development of the pyruvic acid reaction for onion pungency measurement. © 2015 Society of Chemical Industry.

Facile Separation of 5-O-Galloylquinic Acid from Chinese Green Tea Extract using Mesoporous Zirconium Phosphate.

PubMed

Ma, Yilong; Shang, Yafang; Zhu, Danye; Wang, Caihong; Zhong, Zhifeng; Xu, Ziyang

2016-05-01

5-O-Galloylquinic acid from green tea and other plants is attracting increasing attention for its antioxidant and antileishmanial bioactivities. It is always isolated using a silica column, a Sephadex column and high-performance liquid chromatography (HPLC) methods, which are either laborious or instrument dependent. To develop a new method to easily separate 5-O-galloylquinic acid. Mesoporous zirconium phosphate (m-ZrP) was prepared to conveniently separate 5-O-galloylquinic acid from Chinese green tea extract, and the target compound was easily obtained by simple steps of adsorption, washing and desorption. The effects of the green tea extraction conditions, extract concentrations, and m-ZrP adsorption/desorption dynamics on the 5-O-galloylquinic acid separation were evaluated. 5-O-Galloylquinic acid that was separated from a 70% ethanol extract of green tea was of moderate HPLC purity (92%) and recovery (88%), and an increased non-specific binding of epigallocatechin gallate (EGCG) on m-ZrP was observed in the diluted tea extract. The times for maximal adsorption of 5-O-galloylquinic acid in 70% ethanol extract and maximal desorption of 5-O-galloylquinic acid in 0.4% phosphoric acid solution were confirmed as 7 h and 5 h, respectively. A facile method to separate 5-O-galloylquinic acid from Chinese green tea extract using m-ZrP was established. Copyright © 2016 John Wiley & Sons, Ltd. Copyright © 2016 John Wiley & Sons, Ltd.

Evaluation of methods of determining humic acids in nucleic acid samples for molecular biological analysis.

PubMed

Wang, Yong; Fujii, Takeshi

2011-01-01

It is important in molecular biological analyses to evaluate contamination of co-extracted humic acids in DNA/RNA extracted from soil. We compared the sensitivity of various methods for measurement of humic acids, and influences of DNA/RNA and proteins on the measurement. Considering the results, we give suggestions as to choice of methods for measurement of humic acids in molecular biological analyses.

Simultaneous quantification of eight organic acid components in Artemisia capillaris Thunb (Yinchen) extract using high-performance liquid chromatography coupled with diode array detection and high-resolution mass spectrometry.

PubMed

Yu, Fangjun; Qian, Hao; Zhang, Jiayu; Sun, Jie; Ma, Zhiguo

2018-04-01

We aim to determine the chemical constituents of Yinchen extract and Yinchen herbs using high-performance liquid chromatography coupled with diode array detection and high-resolution mass spectrometry. The method was developed to analyze of eight organic acid components of Yinchen extract (including neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, 1,3-dicaffeoylquinic acid, 3,4-dicaffeoylquinic acid, 3,5-dicaffeoylquinic acid and 4,5-dicaffeoylquinic acid). The separation was conducted using an Agilent TC-C18 column with acetonitrile - 0.2% formic acid solution as the mobile phases under gradient elution. The analytical method was fully validated in terms of linearity, sensitivity, precision, repeatability as well as recovery, and subsequently the method was performed for the quantitative assessment of Yinchen extracts and Yinchen herbs. In addition, the changes of selected markers were studied when Yinchen herbs decocting in water and isomerization occurred between the chlorogenic acids. The proposed method enables both qualitative and quantitative analyses and could be developed as a new tool for the quality evaluation of Yinchen extract and Yinchen herbs. The changes of selected markers in water decoction process could give us some novel idea when studying the link between substances and drug efficacy. Copyright © 2017. Published by Elsevier B.V.

Comparison of methods for extracting kafirin proteins from sorghum distillers dried grains with solubles.

PubMed

Wang, Ying; Tilley, Michael; Bean, Scott; Sun, X Susan; Wang, Donghai

2009-09-23

Use of coproducts generated during fermentation is important to the overall economics of biofuel production. The main coproduct from grain-based ethanol production is distillers dried grains with solubles (DDGS). High in protein, DDGS is a potential source of protein for many bioindustrial applications such as adhesives and resins. The objective of this research was to characterize the composition as well as chemical and physical properties of kafirin proteins from sorghum DDGS with various extraction methods including use of acetic acid, HCl-ethanol and NaOH-ethanol under reducing conditions. Extraction conditions affected purity and thermal properties of the extracted kafirin proteins. Extraction yields of 44.2, 24.2, and 56.8% were achieved by using acetic acid, HCl-ethanol and NaOH-ethanol, respectively. Acetic acid and NaOH-ethanol produced protein with higher purity than kafirins extracted with the HCl-ethanol protocol. The acetic acid extraction protocol produced protein with the highest purity, 98.9%. Several techniques were used to evaluate structural, molecular and thermal properties of kairin extracts. FTIR showed alpha-helix dominated in all three samples, with only a small portion of beta-sheet present. Electrophoresis results showed alpha(1), alpha(2) band and beta kafirins were present in all three extracts. Glass transition peaks of the extracts were shown by DSC to be approximately 230 degrees C. Kafirin degraded at 270-290 degrees C. Size exclusion chromatography revealed that the acetic acid and HCl-ethanol based extraction methods tended to extract more high molecular weight protein than the NaOH-ethanol based method. Reversed phase high-performance liquid chromatography showed that the gamma kafirins were found only in extracts from the NaOH-ethanol extraction method.

Role of modifier in microwave assisted extraction of oleanolic acid from Gymnema sylvestre: application of green extraction technology for botanicals.

PubMed

Mandal, Vivekananda; Dewanjee, Saikat; Mandal, Subhash C

2009-08-01

This work highlights the development of a green extraction technology for botanicals with the use of microwave energy. Taking into consideration the extensive time involved in conventional extraction methods, coupled with usage of large volumes of organic solvent and energy resources, an ecofriendly green method that can overcome the above problems has been developed. The work compares the effect of sample pretreatment with untreated sample for improved yield of oleanolic acid from Gymnema sylvestre leaves. The pretreated sample with water produced 0.71% w/w oleanolic acid in one extraction cycle with 500 W microwave power, 25 mL methanol and only an 8 min extraction time. On the other hand, a conventional heat reflux extraction for 6 hours could produce only 0.62% w/w oleanolic acid. The detailed mechanism of extraction has been studied through scanning electron micrographs. The environmental impact of the proposed green method has also been evaluated.

Analysis of non-esterified fatty acids in human samples by solid-phase-extraction and gas chromatography/mass spectrometry.

PubMed

Kopf, Thomas; Schmitz, Gerd

2013-11-01

The determination of the fatty acid (FA) profile of lipid classes is essential for lipidomic analysis. We recently developed a GC/MS-method for the analysis of the FA profile of total FAs, i.e. the totality of bound and unbound FAs, in any given biological sample (TOFAs). Here, we present a method for the analysis of non-esterified fatty acids (NEFAs) in biological samples, i.e. the fraction that is present as extractable free fatty acids. Lipid extraction is performed according to Dole using 80/20 2-propanol/n-hexane (v/v), with 0.1% H2SO4. The fatty acid-species composition of this NEFA-fraction is determined as FAME after derivatization with our GC/MS-method on a BPX column (Shimadzu). Validation of the NEFA-method presented was performed in human plasma samples. The validated method has been used with human plasma, cells and tissues, as well as mammalian body fluids and tissue samples. The newly developed solid-phase-extraction (SPE)-GC-MS method allows the rapid separation of the NEFA-fraction from a neutral lipid extract of plasma samples. As a major advantage compared to G-FID-methods, GC-MS allows the use of stable isotope labeled fatty acid precursors to monitor fatty acid metabolism. Copyright © 2013 Elsevier B.V. All rights reserved.

Effects of different biomass drying and lipid extraction methods on algal lipid yield, fatty acid profile, and biodiesel quality.

PubMed

Hussain, Javid; Liu, Yan; Lopes, Wilson A; Druzian, Janice I; Souza, Carolina O; Carvalho, Gilson C; Nascimento, Iracema A; Liao, Wei

2015-03-01

Three lipid extraction methods of hexane Soxhlet (Sox-Hex), Halim (HIP), and Bligh and Dyer (BD) were applied on freeze-dried (FD) and oven-dried (OD) Chlorella vulgaris biomass to evaluate their effects on lipid yield, fatty acid profile, and algal biodiesel quality. Among these three methods, HIP was the preferred one for C. vulgaris lipid recovery considering both extraction efficiency and solvent toxicity. It had the highest lipid yields of 20.0 and 22.0% on FD and OD biomass, respectively, with corresponding neutral lipid yields of 14.8 and 12.7%. The lipid profiling analysis showed that palmitic, oleic, linoleic, and α-linolenic acids were the major fatty acids in the algal lipids, and there were no significant differences on the amount of these acids between different drying and extraction methods. Correlative models applied to the fatty acid profiles concluded that high contents of palmitic and oleic acids in algal lipids contributed to balancing the ratio of saturated and unsaturated fatty acids and led to a high-quality algal biodiesel.

Microbial process for the preparation of acetic acid as well as solvent for its extraction from the fermentation broth

DOEpatents

Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

2006-07-11

A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. This solvent is substantially devoid of mono-alkyl amines and alcohols. Solvent mixtures formed of such a modified solvent with a desired cosolvent, preferably a low boiling hydrocarbon which forms an azeotrope with water are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

Microbial process for the preparation of acetic acid as well as solvent for its extraction from the fermentation broth

DOEpatents

Gaddy, James L.; Clausen, Edgar C.; Ko, Ching-Whan; Wade, Leslie E.; Wikstrom, Carl V.

2002-01-01

A modified water-immiscible solvent useful in the extraction of acetic acid from aqueous streams is a substantially pure mixture of isomers of highly branched di-alkyl amines. This solvent is substantially devoid of mono-alkyl amines and alcohols. Solvent mixtures formed of such a modified solvent with a desired cosolvent, preferably a low boiling hydrocarbon which forms an azeotrope with water are useful in the extraction of acetic acid from aqueous gaseous streams. An anaerobic microbial fermentation process for the production of acetic acid employs such solvents, under conditions which limit amide formation by the solvent and thus increase the efficiency of acetic acid recovery. Methods for the direct extraction of acetic acid and the extractive fermentation of acetic acid also employ the modified solvents and increase efficiency of acetic acid production. Such increases in efficiency are also obtained where the energy source for the microbial fermentation contains carbon dioxide and the method includes a carbon dioxide stripping step prior to extraction of acetic acid in solvent.

Comparison of GC-MS and FTIR methods for quantifying naphthenic acids in water samples.

PubMed

Scott, Angela C; Young, Rozlyn F; Fedorak, Phillip M

2008-11-01

The extraction of bitumen from the oil sands in Canada releases toxic naphthenic acids into the process-affected waters. The development of an ideal analytical method for quantifying naphthenic acids (general formula C(n)H(2n+Z)O(2)) has been impeded by the complexity of these mixtures and the challenges of differentiating naphthenic acids from other naturally-occurring organic acids. The oil sands industry standard FTIR method was compared with a newly-developed GC-MS method. Naphthenic acids concentrations were measured in extracts of surface and ground waters from locations within the vicinity of and away from the oil sands deposits and in extracts of process-affected waters. In all but one case, FTIR measurements of naphthenic acids concentrations were greater than those determined by GC-MS. The detection limit of the GC-MS method was 0.01 mg L(-1) compared to 1 mg L(-1) for the FTIR method. The results indicated that the GC-MS method is more selective for naphthenic acids, and that the FTIR method overestimates their concentrations.

Effects of aerosol formulation to amino acids and fatty acids contents in Haruan extract.

PubMed

Febriyenti; Bai-Baie, Saringat Bin; Laila, Lia

2012-01-01

Haruan (Channa striatus) extract was formulated to aerosol for wound and burn treatment. Haruan extract is containing amino acids and fatty acids that important for wound healing process. The purpose of this study is to observe the effect of formulation and other excipients in the formula to amino acids and fatty acids content in Haruan extract before and after formulated into aerosol. Precolumn derivatization with 6-aminoquinolyl-N-hydroxysuccinimidyl carbamate (AQC) method is used for amino acids analysis. Fatty acids in Haruan extract were esterified using transesterification method to form FAMEs before analyzed using GC. Boron trifluoride-methanol reagent is used for transesterification. Tyrosine and methionine concentrations were different after formulated. The concentrations were decrease. There are six fatty acids have amount that significantly different after formulated into concentrate and aerosol. Contents of these fatty acids were increase. Generally, fatty acids which had content increased after formulated were the long-chain fatty acids. This might be happen because of chain extension process. Saponification and decarboxylation would give the chain extended product. Therefore contents of long-chain fatty acids were increase. Generally, the aerosol formulation did not affect the amino acids concentrations in Haruan extract while some long-chain fatty acids concentrations were increase after formulated into concentrate and aerosol.

Graphene oxide for solid-phase extraction of bioactive phenolic acids.

PubMed

Hou, Xiudan; Wang, Xusheng; Sun, Yingxin; Wang, Licheng; Guo, Yong

2017-05-01

A solid-phase extraction (SPE) method for the efficient analysis of trace phenolic acids (PAs, caffeic acid, ferulic acid, protocatechuic acid, cinnamic acid) in urine was established. In this work, a graphene oxide (GO) coating was grafted onto pure silica to be investigated as SPE material. The prepared GO surface had a layered and wrinkled structure that was rough and well organized, which could provide more open adsorption sites. Owing to its hydrophilicity and polarity, GO showed higher extraction efficiency toward PAs than reduced GO did, in agreement with the theoretical calculation results performed by Gaussian 09 software. The adsorption mechanism of PAs on GO@Sil was also investigated through static state and kinetic state adsorption experiments, which showed a monolayer surface adsorption. Extraction capacity of the as-prepared material was optimized using the response surface methodology. Under the optimized conditions, the as-established method provided wide linearity range (2-50 μg L -1 for protocatechuic acid and 1-50 μg L -1 for caffeic acid, ferulic acid, and cinnamic acid) and low limits of detection (0.25-1 μg L -1 ). Finally, the established method was applied for the analysis of urine from two healthy volunteers. The results indicate that the prepared material is a practical, cost-effective medium for the extraction and determination of phenolic acids in complex matrices. Graphical Abstract A graphene oxide coating was grafted onto pure silica as the SPE material for the extraction of phenolic acids in urines and the extraction mechanism was also mainly investigated.

Selective extraction of metal ions with polymeric extractants by ion exchange/redox

DOEpatents

Alexandratos, Spiro D.

1987-01-01

The specification discloses a method for the extraction of metal ions having a reduction potential of above about +0.3 from an aqueous solution. The method includes contacting the aqueous solution with a polymeric extractant having primary phosphinic acid groups, secondary phosphine oxide groups, or both phosphinic acid and phosphine oxide groups.

Method and apparatus for back-extracting metal chelates

DOEpatents

Wai, Chien M.; Smart, Neil G.; Lin, Yuehe

1998-01-01

A method of extracting metal and metalloid species from a solid or liquid substrate using a supercritical fluid solvent containing one or more chelating agents followed by back-extracting the metal and metalloid species from the metal and metalloid chelates formed thereby. The back-extraction acidic solution is performed utilizing an acidic solution. Upon sufficient exposure of the metal and metalloid chelates to the acidic solution, the metal and metalloid species are released from the chelates into the acid solution, while the chelating agent remains in the supercritical fluid solvent. The chelating agent is thereby regenerated and the metal and metalloid species recovered.

Design of experiments for amino acid extraction from tobacco leaves and their subsequent determination by capillary zone electrophoresis.

PubMed

Hodek, Ondřej; Křížek, Tomáš; Coufal, Pavel; Ryšlavá, Helena

2017-03-01

In this study, we optimized a method for the determination of free amino acids in Nicotiana tabacum leaves. Capillary electrophoresis with contactless conductivity detector was used for the separation of 20 proteinogenic amino acids in acidic background electrolyte. Subsequently, the conditions of extraction with HCl were optimized for the highest extraction yield of the amino acids because sample treatment of plant materials brings some specific challenges. Central composite face-centered design with fractional factorial design was used in order to evaluate the significance of selected factors (HCl volume, HCl concentration, sonication, shaking) on the extraction process. In addition, the composite design helped us to find the optimal values for each factor using the response surface method. The limits of detection and limits of quantification for the 20 proteinogenic amino acids were found to be in the order of 10 -5 and 10 -4  mol l -1 , respectively. Addition of acetonitrile to the sample was tested as a method commonly used to decrease limits of detection. Ambiguous results of this experiment pointed out some features of plant extract samples, which often required specific approaches. Suitability of the method for metabolomic studies was tested by analysis of a real sample, in which all amino acids, except for L-methionine and L-cysteine, were successfully detected. The optimized extraction process together with the capillary electrophoresis method can be used for the determination of proteinogenic amino acids in plant materials. The resulting inexpensive, simple, and robust method is well suited for various metabolomic studies in plants. As such, the method represents a valuable tool for research and practical application in the fields of biology, biochemistry, and agriculture.

Development and validation of an HPLC-method for determination of free and bound phenolic acids in cereals after solid-phase extraction.

PubMed

Irakli, Maria N; Samanidou, Victoria F; Biliaderis, Costas G; Papadoyannis, Ioannis N

2012-10-01

Whole cereal grains are a good source of phenolic acids associated with reduced risk of chronic diseases. This paper reports the development and validation of a high-performance liquid chromatography-diode array detection (HPLC-DAD) method for the determination of phenolic acids in cereals in either free or bound form. Extraction of free phenolic acids and clean-up was performed by an optimised solid-phase extraction (SPE) protocol on Oasis HLB cartridges using aqueous methanol as eluant. The mean recovery of analytes ranged between 84% and 106%. Bound phenolic acids were extracted using alkaline hydrolysis with mean recoveries of 80-95%, except for gallic acid, caffeic acid and protocatechuic acid. Both free and bound phenolic extracts were separated on a Nucleosil 100 C18 column, 5 μm (250 mm × 4.6 mm) thermostated at 30 °C, using a linear gradient elution system consisting of 1% (v/v) acetic acid in methanol. Method validation was performed by means of linearity, accuracy, intra-day and inter-day precision and sensitivity. Detection limits ranged between 0.13 and 0.18 μg/g. The method was applied to the analysis of free and bound phenolic acids contents in durum wheat, bread wheat, barley, oat, rice, rye, corn and triticale. Copyright © 2012 Elsevier Ltd. All rights reserved.

Investigation of Pu(IV)-acetohydroxamic acid complex by solvent extraction with di(2-ethylhexyl) phosphoric acid

NASA Astrophysics Data System (ADS)

Brown, M. Alex; Paulenova, Alena; Tkac, Peter

2010-03-01

The stability constant of the Pu(IV)-acetohydroxamic acid complex Pu(AHA)3+ at 1 M ionic strength (pH = 0) has been investigated by method of solvent extraction. Di(2-ethylhexyl) phosphoric acid (HDEHP) was used to extract Pu(IV) from perchloric and nitric acid media at various AHA concentrations. Distribution ratios over a range of ligand concentrations were used in conjunction with graphical methods to obtain logβ1 = 14.3 ± 0.03 in perchloric acid. The stability constant determined from solutions in nitric acid was excluded because of the uncertainty in plutonium speciation.

An automated method for the analysis of phenolic acids in plasma based on ion-pairing micro-extraction coupled on-line to gas chromatography/mass spectrometry with in-liner derivatisation.

PubMed

Peters, Sonja; Kaal, Erwin; Horsting, Iwan; Janssen, Hans-Gerd

2012-02-24

A new method is presented for the analysis of phenolic acids in plasma based on ion-pairing 'Micro-extraction in packed sorbent' (MEPS) coupled on-line to in-liner derivatisation-gas chromatography-mass spectrometry (GC-MS). The ion-pairing reagent served a dual purpose. It was used both to improve extraction yields of the more polar analytes and as the methyl donor in the automated in-liner derivatisation method. In this way, a fully automated procedure for the extraction, derivatisation and injection of a wide range of phenolic acids in plasma samples has been obtained. An extensive optimisation of the extraction and derivatisation procedure has been performed. The entire method showed excellent repeatabilities of under 10% and linearities of 0.99 or better for all phenolic acids. The limits of detection of the optimised method for the majority of phenolic acids were 10ng/mL or lower with three phenolic acids having less-favourable detection limits of around 100 ng/mL. Finally, the newly developed method has been applied in a human intervention trial in which the bioavailability of polyphenols from wine and tea was studied. Forty plasma samples could be analysed within 24h in a fully automated method including sample extraction, derivatisation and gas chromatographic analysis. Copyright © 2011 Elsevier B.V. All rights reserved.

Comparison of Composition and Anticaries Effect of Galla Chinensis Extracts with Different Isolation Methods

PubMed Central

Huang, Xuelian; Deng, Meng; Liu, Mingdong; Cheng, Lei; Exterkate, R.A.M.; Li, Jiyao; Zhou, Xuedong; Ten Cate, Jacob. M.

2017-01-01

Objectives: Galla chinensis water extract (GCE) has been demonstrated to inhibit dental caries by favorably shifting the demineralization/remineralization balance of enamel and inhibiting the biomass and acid formation of dental biofilm. The present study focused on the comparison of composition and anticaries effect of Galla chinensis extracts with different isolation methods, aiming to improve the efficacy of caries prevention. Methods: The composition of water extract (GCE), ethanol extract (eGCE) and commercial tannic acid was compared. High performance liquid chromatography coupled to electrospray ionization-time of flight-mass spectrometry (HPLC-ESI-TOF-MS) analysis was used to analyze the main ingredients. In vitro pH-cycling regime and polymicrobial biofilms model were used to assess the ability of different Galla chinensis extracts to inhibit enamel demineralization, acid formation and biofilm formation. Results: All the GCE, eGCE and tannic acid contained a high level of total phenolics. HPLC-ESI-TOF-MS analysis showed that the main ingredients of GCE were gallic acid (GA), while eGCE mainly contained 4-7 galloylglucopyranoses (GGs) and tannic acid mainly contained 5-10 GGs. Furthermore, eGCE and tannic acid showed a better effect on inhibiting enamel demineralization, acid formation and biofilm formation compared to GCE. Conclusions: Galla chinensis extracts with higher tannin content were suggested to have higher potential to prevent dental caries. PMID:28979574

Microwave-assisted extraction with water for fast extraction and simultaneous RP-HPLC determination of phenolic acids in radix Salviae Miltiorrhizae.

PubMed

Fang, Xinsheng; Wang, Jianhua; Zhou, Hongying; Jiang, Xingkai; Zhu, Lixiang; Gao, Xin

2009-07-01

An optimized microwave-assisted extraction method using water (MAE-W) as the extractant and an efficient HPLC analysis method were first developed for the fast extraction and simultaneous determination of D(+)-(3,4-dihydroxyphenyl) lactic acid (Dla), salvianolic acid B (SaB), and lithospermic acid (La) in radix Salviae Miltiorrhizae. The key parameters of MAE-W were optimized. It was found that the degradation of SaB was inhibited when using the optimized MAE-W and the stable content of Dla, La, and SaB in danshen was obtained. Furthermore, compared to the conventional extraction methods, the proposed MAE-W is a more rapid method with higher yield and lower solvent consumption with a reproducibility (RSD <6%). In addition, using water as extractant is safe and helpful for environment protection, which could be referred to as green extraction. The separation and quantitative determination of the three compounds was carried out by a developed reverse-phase high-performance liquid chromatographic (RP-HPLC) method with UV detection. Highly efficient separation was obtained using gradient solvent system. The optimized HPLC analysis method was validated to have specificity, linearity, precision, and accuracy. The results indicated that MAE-W followed by HPLC-UV determination is an appropriate alternative to previously proposed method for quality control of radix Salviae Miltiorrhizae.

Influence of Humic Acids Extracted from Peat by Different Methods on Functional Activity of Macrophages in Vitro.

PubMed

Trofimova, E S; Zykova, M V; Ligacheva, A A; Sherstoboev, E Y; Zhdanov, V V; Belousov, M V; Yusubov, M S; Krivoshchekov, S V; Danilets, M G; Dygai, A M

2017-04-01

We studied activation of macrophages with humic acids extracted from peat of large deposits in the Tomsk region by two extraction methods: by hydroxide or sodium pyrophosphate. Humic acid of lowland peat types containing large amounts of aromatic carbon, phenolic and alcohol groups, carbohydrate residues and ethers, irrespectively of the extraction methods contained LPS admixture that probably determines their activating properties. Humic acid of upland peat types characterized by high content of carbonyl, carboxyl, and ester groups enhance NO production and reduce arginase expression, but these effects were minimized when sodium hydroxide was used as an extraction solvent. Pyrophosphate samples of the upland peat types were characterized by aromaticity and diversity of functional groups and have a significant advantage because of they induce specific endotoxin-independent stimulating action on antigen presenting cells.

SIMPLE METHOD FOR THE EXTRACTION OF PHOTOPIGMENTS AND MYCOSPORINE-LIKE AMINO ACIDS (MAAS) FROM SYMBIODINIUM SPP.

EPA Science Inventory

Numerous extraction methods have been developed and used in the quantitation of both photopigments and mycosporine amino acids (MAAs) found in Symbiodinium sp. and zooanthellate metazoans. We have development of a simple, mild extraction procedure using methanol, which when coupl...

Development of a rapid LC-DAD/FLD method for the simultaneous determination of auxins and abscisic acid in plant extracts.

PubMed

Bosco, Renato; Caser, Matteo; Vanara, Francesca; Scariot, Valentina

2013-11-20

Plant hormones play a crucial role in controlling plant growth and development. These groups of naturally occurring substances trigger physiological processes at very low concentrations, which mandate sensitive techniques for their quantitation. This paper describes a method to quantify endogenous (±)-2-cis-4-trans-abscisic acid, indole-3-acetic acid, indole-3-propionic acid, and indole-3-butyric acid. The method combines high-performance liquid chromatography (HPLC) with diode array and fluorescence detection in a single run. Hybrid tea rose 'Monferrato' matrices (leaves, petals, roots, seeds, androecium, gynoecium, and pollen) were used as references. Rose samples were separated and suspended in extracting methanol, after which (±)-2-cis-4-trans-abscisic acid and auxins were extracted by solvent extraction. Sample solutions were added first to cation solid phase extraction (SPE) cartridges and the eluates to anion SPE cartridges. The acidic hormones were bound to the last column and eluted with 5% phosphoric acid in methanol. Experimental results showed that this approach can be successfully applied to real samples and that sample preparation and total time for routine analysis can be greatly reduced.

High-resolution gas chromatography/mas spectrometry method for characterization and quantitative analysis of ginkgolic acids in ginkgo biloba plants, extracts, and dietary supplements

USDA-ARS?s Scientific Manuscript database

A high resolution GC/MS with Selected Ion Monitor (SIM) method focusing on the characterization and quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba L. plant materials, extracts and commercial products was developed and validated. The method involved sample extraction with (1:1) meth...

Comparison of the ion exclusion chromatographic method with the Monier-Williams method for determination of total sulfite in foods.

PubMed

Kim, H J

1989-01-01

Experimental data comparing the alkali extraction/ion exclusion chromatographic method with the Monier-Williams method for determination of total sulfite are presented in (a) enzymatic and nonenzymatic browning systems, (b) vegetables containing naturally occurring sulfite, and (c) a carbohydrate-type food additive, erythorbic acid. Excellent agreement, with a linear correlation coefficient of 0.99, was observed in fresh potato samples homogenized with sulfite and allowed to react for different time intervals (enzymatic browning system). A good overall correlation was observed in dehydrated, sulfited apple samples heated for different times (nonenzymatic browning system); however, as heating time increased, higher results were obtained by the Monier-Williams method than by the alkali extraction/ion exclusion chromatographic method. The results of determining sulfite in the alkali trapping solution following acid distillation or acid treatment without heat suggested that this deviation was due to a fraction of sulfite bound to the browning reaction products in such a way that it was released by acid distillation but not by alkali extraction or acid treatment without heat. Similar behavior was demonstrated in cabbage with naturally occurring sulfite, which was released by acid distillation but not by alkali extraction or acid treatment without heat. The ion exclusion chromatographic method could overcome interference by the volatile caramelization reaction products in the Monier-Williams determination of erythorbic acid.

Optimization of ultrasound-assisted extraction of crude oil from winter melon (Benincasa hispida) seed using response surface methodology and evaluation of its antioxidant activity, total phenolic content and fatty acid composition.

PubMed

Bimakr, Mandana; Rahman, Russly Abdul; Taip, Farah Saleena; Adzahan, Noranizan Mohd; Sarker, Md Zaidul Islam; Ganjloo, Ali

2012-10-08

In the present study, ultrasound-assisted extraction of crude oil from winter melon seeds was investigated through response surface methodology (RSM). Process variables were power level (25-75%), temperature (45-55 °C) and sonication time (20-40 min). It was found that all process variables have significant (p < 0.05) effects on the response variable. A central composite design (CCD) was used to determine the optimum process conditions. Optimal conditions were identified as 65% power level, 52 °C temperature and 36 min sonication time for maximum crude yield (108.62 mg-extract/g-dried matter). The antioxidant activity, total phenolic content and fatty acid composition of extract obtained under optimized conditions were determined and compared with those of oil obtained by the Soxhlet method. It was found that crude extract yield (CEY) of ultrasound-assisted extraction was lower than that of the Soxhlet method, whereas antioxidant activity and total phenolic content of the extract obtained by ultrasound-assisted extraction were clearly higher than those of the Soxhlet extract. Furthermore, both extracts were rich in unsaturated fatty acids. The major fatty acids of the both extracts were linoleic acid and oleic acid.

Simultaneous Determination and Pharmacokinetic Comparisons of Multi-Ingredients after Oral Administration of Radix Salviae Miltiorrhizae Extract, Hawthorn Extract, and a Combination of Both Extracts to Rats

PubMed Central

Liu, Yu-Qiang; Cai, Qian; Liu, Chang; Bao, Feng-Wei; Zhang, Zhen-Qiu

2014-01-01

A simple and sensitive HPLC method was developed for simultaneous determination of danshensu (DSS), rosmarinic acid (RA), lithospermic acid (LA), salvianolic acid B (SAB), and hyperoside (HP) in rat plasma. This method validated was successfully applied to the pharmacokinetic study of the main active ingredients after oral administration of Radix Salviae Miltiorrhizae extract (SME), hawthorn extract (HTE), and a combination of both extracts (2.5 : 1) to rats. The results indicated that there have been great differences in pharmacokinetics between a single extract and a combination of both extracts. A combination of both extracts can enhance their bioavailabilities and delay the elimination of SAB and DSS in rats. PMID:24660090

Method and apparatus for back-extracting metal chelates

DOEpatents

Wai, C.M.; Smart, N.G.; Lin, Y.

1998-08-11

A method is described for extracting metal and metalloid species from a solid or liquid substrate using a supercritical fluid solvent containing one or more chelating agents followed by back-extracting the metal and metalloid species from the metal and metalloid chelates formed thereby. The back-extraction acidic solution is performed utilizing an acidic solution. Upon sufficient exposure of the metal and metalloid chelates to the acidic solution, the metal and metalloid species are released from the chelates into the acid solution, while the chelating agent remains in the supercritical fluid solvent. The chelating agent is thereby regenerated and the metal and metalloid species recovered. 3 figs.

Effective protein extraction protocol for proteomics studies of Jerusalem artichoke leaves.

PubMed

Zhang, Meide; Shen, Shihua

2013-07-01

Protein extraction is a crucial step for proteomics studies. To establish an effective protein extraction protocol suitable for two-dimensional electrophoresis (2DE) analysis in Jerusalem artichoke (Helianthus tuberosus L.), three different protein extraction methods-trichloroacetic acid/acetone, Mg/NP-40, and phenol/ammonium acetate-were evaluated using Jerusalem artichoke leaves as source materials. Of the three methods, trichloroacetic acid/acetone yielded the best protein separation pattern and highest number of protein spots in 2DE analysis. Proteins highly abundant in leaves, such as Rubisco, are typically problematic during leaf 2DE analysis, however, and this disadvantage was evident using trichloroacetic acid/acetone. To reduce the influence of abundant proteins on the detection of low-abundance proteins, we optimized the trichloroacetic acid/acetone method by incorporating a PEG fractionation approach. After optimization, 363 additional (36.2%) protein spots were detected on the 2DE gel. Our results suggest that trichloroacetic acid/acetone method is a better protein extraction technique than Mg/NP-40 and phenol/ammonium acetate in Jerusalem artichoke leaf 2DE analysis, and that trichloroacetic acid/acetone method combined with PEG fractionation procedure is the most effective approach for leaf 2DE analysis of Jerusalem artichoke. © 2013 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Ultrasound-Assisted Extraction of Carnosic Acid and Rosmarinic Acid Using Ionic Liquid Solution from Rosmarinus officinalis

PubMed Central

Zu, Ge; Zhang, Rongrui; Yang, Lei; Ma, Chunhui; Zu, Yuangang; Wang, Wenjie; Zhao, Chunjian

2012-01-01

Ionic liquid based, ultrasound-assisted extraction was successfully applied to the extraction of phenolcarboxylic acids, carnosic acid and rosmarinic acid, from Rosmarinus officinalis. Eight ionic liquids, with different cations and anions, were investigated in this work and [C8mim]Br was selected as the optimal solvent. Ultrasound extraction parameters, including soaking time, solid–liquid ratio, ultrasound power and time, and the number of extraction cycles, were discussed by single factor experiments and the main influence factors were optimized by response surface methodology. The proposed approach was demonstrated as having higher efficiency, shorter extraction time and as a new alternative for the extraction of carnosic acid and rosmarinic acid from R. officinalis compared with traditional reference extraction methods. Ionic liquids are considered to be green solvents, in the ultrasound-assisted extraction of key chemicals from medicinal plants, and show great potential. PMID:23109836

Comparative assessment of the methods for exchangeable acidity measuring

NASA Astrophysics Data System (ADS)

Vanchikova, E. V.; Shamrikova, E. V.; Bespyatykh, N. V.; Zaboeva, G. A.; Bobrova, Yu. I.; Kyz"yurova, E. V.; Grishchenko, N. V.

2016-05-01

A comparative assessment of the results of measuring the exchangeable acidity and its components by different methods was performed for the main mineral genetic horizons of texturally-differentiated gleyed and nongleyed soddy-podzolic and gley-podzolic soils of the Komi Republic. It was shown that the contents of all the components of exchangeable soil acidity determined by the Russian method (with potassium chloride solution as extractant, c(KCl) = 1 mol/dm3) were significantly higher than those obtained by the international method (with barium chloride solution as extractant, c(BaCl2) = 0.1 mol/dm3). The error of the estimate of the concentration of H+ ions extracted with barium chloride solution equaled 100%, and this allowed only qualitative description of this component of the soil acidity. In the case of the extraction with potassium chloride, the error of measurements was 50%. It was also shown that the use of potentiometric titration suggested by the Russian method overestimates the results of soil acidity measurement caused by the exchangeable metal ions (Al(III), Fe(III), and Mn(II)) in comparison with the atomic emission method.

Combining cationic and anionic mixed-mode sorbents in a single cartridge to extract basic and acidic pharmaceuticals simultaneously from environmental waters.

PubMed

Salas, Daniela; Borrull, Francesc; Fontanals, Núria; Marcé, Rosa Maria

2018-01-01

The aim of the present study is to broaden the applications of mixed-mode ion-exchange solid-phase extraction sorbents to extract both basic and acidic compounds simultaneously by combining the sorbents in a single cartridge and developing a simplified extraction procedure. Four different cartridges containing negative and positive charges in the same configuration were evaluated and compared to extract a group of basic, neutral, and acidic pharmaceuticals selected as model compounds. After a thorough optimization of the extraction conditions, the four different cartridges showed to be capable of retaining basic and acidic pharmaceuticals simultaneously through ionic interactions, allowing the introduction of a washing step with 15 mL methanol to eliminate interferences retained by hydrophobic interactions. Using the best combined cartridge, a method was developed, validated, and further applied to environmental waters to demonstrate that the method is promising for the extraction of basic and acidic compounds from very complex samples.

Molecular docking and ex vivo and in vitro anticholinesterase activity studies of Salvia sp. and highlighted rosmarinic acid.

PubMed

Demirezer, Lütfiye Ömür; Gürbüz, Perihan; Kelicen Uğur, Emine Pelin; Bodur, Mine; Özenver, Nadire; Uz, Ayse; Güvenalp, Zühal

2015-01-01

To evaluate acetylcholinesterase (AChE) inhibitory activity and antioxidant capacity of the major molecule from Salvia sp., rosmarinic acid, as a drug candidate molecule for treatment of Alzheimer disease (AD). The AChE inhibitory activity of different extracts from Salvia trichoclada, Salvia verticillata, and Salvia fruticosa was determined by the Ellman and isolated guinea pig ileum methods, and the antioxidant capacity was determined with DPPH. The AChE inhibitory activity of the major molecule rosmarinic acid was determined by in silico docking and isolated guinea pig ileum methods. The methanol extract of Salvia trichoclada showed the highest inhibition on AChE. The same extract and rosmarinic acid showed significant contraction responses on isolated guinea pig ileum. All the extracts and rosmarinic acid showed high radical scavenging capacities. Docking results of rosmarinic acid showed high affinity to the selected target, AChE. In this study in vitro and ex vivo studies and in silico docking research of rosmarinic acid were used simultaneously for the first time. Rosmarinic acid showed promising results in all the methods tested.

System and method for conditioning a hardwood pulp liquid hydrolysate

DOEpatents

Waite, Darrell M; Arnold, Richard; St. Pierre, James; Pendse, Hemant P; Ceckler, William H

2013-12-17

A system and method for hardwood pulp liquid hydrolysate conditioning includes a first evaporator receives a hardwood mix extract and outputting a quantity of vapor and extract. A hydrolysis unit receives the extract, hyrolyzes and outputs to a lignin separation device, which separates and recovers a quantity of lignin. A neutralization device receives extract from the lignin separation device and a neutralizing agent, producing a mixture of solid precipitate and a fifth extract. The solid precipitate is removed from the fifth extract. A second evaporator removes a quantity of acid from the fifth extract in a vapor form. This vapor may be recycled to improve total acid recovery or discarded. A desalination device receives the diluted extract, separates out some of the acid and salt and outputs a desalinated solution.

A comparative evaluation of six principal IgY antibody extraction methods.

PubMed

Ren, Hao; Yang, Wenjing; Thirumalai, Diraviyam; Zhang, Xiaoying; Schade, Rüdiger

2016-03-01

Egg yolk has been considered a promising source of antibodies. Our study was designed to compare six principal IgY extraction methods (water dilution, polyethylene glycol [PEG] precipitation, caprylic acid extraction, chloroform extraction, phenol extraction, and carrageenan extraction), and to assess their relative extraction efficiencies and the purity of the resulting antibodies. The results showed that the organic solvents (chloroform or phenol) minimised the lipid ratio in the egg yolk. The water dilution, PEG precipitation and caprylic acid extraction methods resulted in high yields, and antibodies purified with PEG and carrageenan exhibited high purity. Our results indicate that phenol extraction would be more suitable for preparing high concentrations of IgY for non-therapeutic usage, while the water dilution and carrageenan extraction methods would be more appropriate for use in the preparation of IgY for oral administration. 2016 FRAME.

Combination of graphene oxide-based solid phase extraction and electro membrane extraction for the preconcentration of chlorophenoxy acid herbicides in environmental samples.

PubMed

Tabani, Hadi; Fakhari, Ali Reza; Shahsavani, Abolfath; Behbahani, Mohammad; Salarian, Mani; Bagheri, Akbar; Nojavan, Saeed

2013-07-26

Combination of different extraction methods is an interesting and debatable work in the field of sample preparation. In the current study, for the first time, solid phase extraction combined with electro membrane extraction (SPE-EME) was developed for ultra-preconcentration and determination of chlorophenoxy acid herbicides in environmental samples using capillary electrophoresis (CE). In the mentioned method, first, a 100mL of chlorophenoxy acid herbicides (2-methyl-4-chlorophenoxyacetic acid (MCPA), 2-(2,4-dichlorophenoxy) propanoic acid (2,4-DP) and 2-(4-chloro-2-methylphenoxy) propanoic acid (MCPP)) was passed through a column of graphene oxide as a solid phase, and then the adsorbed herbicides were eluted by 4.0mL of 8% acetic acid (HOAC) in methanol. Then, the elution solvent was evaporated and the herbicides residue was dissolved in 4.0mL of double distilled water (pH 9.0). Afterwards, the herbicides in 4.0mL of the aqueous solution were transferred to an EME glass vial. In the EME step, the herbicides were extracted from the sample solution into the basic acceptor solution (pH 13.0) under electrical potential, which was held inside the lumen of the fiber with 1-octanol as the supported liquid membrane (SLM). Under the optimized conditions, high enrichment factors were obtained in the range of 1950-2000. The limits of quantification (LOQs) and method detection limits (MDLs) were obtained in the range of 1.0-1.5 and 0.3-0.5ngmL(-1), respectively. Finally, the performance of the present method was evaluated for extraction and determination of chlorophenoxy acid herbicides in environmental samples. Copyright © 2013 Elsevier B.V. All rights reserved.

Separation of phenolic acids from sugarcane rind by online solid-phase extraction with high-speed counter-current chromatography.

PubMed

Geng, Ping; Fang, Yingtong; Xie, Ronglong; Hu, Weilun; Xi, Xingjun; Chu, Qiao; Dong, Genlai; Shaheen, Nusrat; Wei, Yun

2017-02-01

Sugarcane rind contains some functional phenolic acids. The separation of these compounds from sugarcane rind is able to realize the integrated utilization of the crop and reduce environment pollution. In this paper, a novel protocol based on interfacing online solid-phase extraction with high-speed counter-current chromatography (HSCCC) was established, aiming at improving and simplifying the process of phenolic acids separation from sugarcane rind. The conditions of online solid-phase extraction with HSCCC involving solvent system, flow rate of mobile phase as well as saturated extent of absorption of solid-phase extraction were optimized to improve extraction efficiency and reduce separation time. The separation of phenolic acids was performed with a two-phase solvent system composed of butanol/acetic acid/water at a volume ratio of 4:1:5, and the developed online solid-phase extraction with HSCCC method was validated and successfully applied for sugarcane rind, and three phenolic acids including 6.73 mg of gallic acid, 10.85 mg of p-coumaric acid, and 2.78 mg of ferulic acid with purities of 60.2, 95.4, and 84%, respectively, were obtained from 150 mg sugarcane rind crude extracts. In addition, the three different elution methods of phenolic acids purification including HSCCC, elution-extrusion counter-current chromatography and back-extrusion counter-current chromatography were compared. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Estimates of Soil Bacterial Ribosome Content and Diversity Are Significantly Affected by the Nucleic Acid Extraction Method Employed

PubMed Central

Wüst, Pia K.; Nacke, Heiko; Kaiser, Kristin; Marhan, Sven; Sikorski, Johannes; Kandeler, Ellen; Daniel, Rolf

2016-01-01

Modern sequencing technologies allow high-resolution analyses of total and potentially active soil microbial communities based on their DNA and RNA, respectively. In the present study, quantitative PCR and 454 pyrosequencing were used to evaluate the effects of different extraction methods on the abundance and diversity of 16S rRNA genes and transcripts recovered from three different types of soils (leptosol, stagnosol, and gleysol). The quality and yield of nucleic acids varied considerably with respect to both the applied extraction method and the analyzed type of soil. The bacterial ribosome content (calculated as the ratio of 16S rRNA transcripts to 16S rRNA genes) can serve as an indicator of the potential activity of bacterial cells and differed by 2 orders of magnitude between nucleic acid extracts obtained by the various extraction methods. Depending on the extraction method, the relative abundances of dominant soil taxa, in particular Actinobacteria and Proteobacteria, varied by a factor of up to 10. Through this systematic approach, the present study allows guidelines to be deduced for the selection of the appropriate extraction protocol according to the specific soil properties, the nucleic acid of interest, and the target organisms. PMID:26896137

Microwave-Assisted Extraction of Oleanolic Acid and Ursolic Acid from Ligustrum lucidum Ait

PubMed Central

Xia, En-Qin; Wang, Bo-Wei; Xu, Xiang-Rong; Zhu, Li; Song, Yang; Li, Hua-Bin

2011-01-01

Oleanolic acid and ursolic acid are the main active components in fruit of Ligustrum lucidum Ait, and possess anticancer, antimutagenic, anti-inflammatory, antioxidative and antiprotozoal activities. In this study, microwave-assisted extraction of oleanolic acid and ursolic acid from Ligustrum lucidum was investigated with HPLC-photodiode array detection. Effects of several experimental parameters, such as type and concentration of extraction solvent, ratio of liquid to material, microwave power, extraction temperature and microwave time, on the extraction efficiencies of oleanolic acid and ursolic acid from Ligustrum lucidum were evaluated. The influence of experimental parameters on the extraction efficiency of ursolic acid was more significant than that of oleanolic acid (p < 0.05). The optimal extraction conditions were 80% ethanol aqueous solution, the ratio of material to liquid was 1:15, and extraction for 30 min at 70 °C under microwave irradiation of 500 W. Under optimal conditions, the yields of oleanolic acid and ursolic acid were 4.4 ± 0.20 mg/g and 5.8 ± 0.15 mg/g, respectively. The results obtained are helpful for the full utilization of Ligustrum lucidum, which also indicated that microwave-assisted extraction is a very useful method for extraction of oleanolic acid and ursolic acid from plant materials. PMID:21954361

Identification of optimum fatty acid extraction methods for two different microalgae Phaeodactylum tricornutum and Haematococcus pluvialis for food and biodiesel applications.

PubMed

Otero, Paz; Saha, Sushanta Kumar; Gushin, Joanne Mc; Moane, Siobhan; Barron, John; Murray, Patrick

2017-07-01

Microalgae have the potential to synthesize and accumulate lipids which contain high value fatty acids intended for nutrition and biodiesel applications. Nevertheless, lipid extraction methods for microalgae cells are not well established and there is not a standard analytical methodology to extract fatty acids from lipid-producing microalgae. In this paper, current lipid extraction procedures employing organic solvents (chloroform/methanol, 2:1 and 1:2, v/v), sodium hypochlorite solution (NaClO), acid-catalysed hot-water extraction and the saponification process [2.5 M KOH/methanol (1:4, v/v)] have been evaluated with two species of microalgae with different types of cell walls. One is a marine diatom, Phaeodactylum tricornutum, and the other a freshwater green microalga, Haematococcus pluvialis. Lipids from all types of extracts were estimated gravimetrically and their fatty acids were quantified by a HPLC equipped with Q-TOF mass spectrometer. Results indicated significant differences both in lipids yield and fatty acids composition. The chloroform and methanol mixture was the most effective extraction solvent for the unsaturated fatty acids such as DPA (C22:05), DHA, (C22:06), EPA (C20:05) and ARA (C20:04). While acid treatments improved the saturated fatty acids (SFAs) yield, especially the short chain SFA, lauric acid (C12:0), whose amount was 64% higher in P. tricornutum and 156% higher in H. pluvialis compared to organic solvent extractions. Graphical abstract ᅟ.

Copigmentation Of Anthocyanin Extract of Purple Sweet Potatoes (Ipomea Batatas L.) Using Ferulic Acid And Tannic Acid

NASA Astrophysics Data System (ADS)

Susanti, I.; Wijaya, H.; Hasanah, F.; Heryani, S.

2018-02-01

Copigmentation is one of the methods to improve the color stability and intensity of anthocyanin extract. This study aimed to do the copigmentation of the anthocyanin extract of purple sweet potato using ferulic acid and tannic acid. The anthocyanin extraction was conducted with distilled water at pH 7 and pH 2 while the copigmentation was conducted by varying the concentration of ferulic acid and tannic acid. The results showed that best anthocyanin extraction method of the purple sweet potato was using distilled water at pH 2. The yield of freeze dried anthocyanin on the extraction with distilled water at pH 2 was 1710 ppm, while the yield when using distilled water at pH 7 was 888 ppm. Ferulic acid and tannic acid can be used for the copigmentation of anthocyanin extract of purple sweet potato by observing the maximum wavelength shift (bathochromic effect, Δλmax) and increase of color intensity (hyperchromic effect, ΔAmax). The bathochromic effect of ferulic acid began to occur at a concentration of 0.01M, while the hypochromic effect on tannic acid occurred at a concentration of 0.005M and remained up to a concentration of 0.02M. The best copigmentation concentration of ferulic acid was 0.015M, while tannic acid was 0.02M. The use of tannic acid 0.02M is recommended compared to ferulic acid 0.015M because with the same bathocromic effect (Δλmaks = 3,9) results hyperchromic effect (ΔA = 0,258) higher by tannic acid.

Extraction of total nucleic acid based on silica-coated magnetic particles for RT-qPCR detection of plant RNA virus/viroid.

PubMed

Sun, Ning; Deng, Congliang; Zhao, Xiaoli; Zhou, Qi; Ge, Guanglu; Liu, Yi; Yan, Wenlong; Xia, Qiang

2014-02-01

In this study, a nucleic acid extraction method based on silica-coated magnetic particles (SMPs) and RT-qPCR assay was developed to detect Arabis mosaic virus (ArMV), Lily symptomless virus (LSV), Hop stunt viroid (HSVd) and grape yellow speckle viroid 1 (GYSVd-1). The amplification sequences of RT-qPCR were reversely transcribed in vitro as RNA standard templates. The standard curves covered six or seven orders of magnitude with a detection limit of 100 copies per each assay. Extraction efficiency of the SMPs method was evaluated by recovering spiked ssRNAs from plant samples and compared to two commercial kits (TRIzol and RNeasy Plant mini kit). Results showed that the recovery rate of SMPs method was comparable to the commercial kits when spiked ssRNAs were extracted from lily leaves, whereas it was two or three times higher than commercial kits when spiked ssRNAs were extracted from grapevine leaves. SMPs method was also used to extract viral nucleic acid from15 ArMV-positive lily leaf samples and 15 LSV-positive lily leaf samples. SMPs method did not show statistically significant difference from other methods on detecting ArMV, but LSV. The SMPs method has the same level of virus load as the TRIzol, and its mean virus load of was 0.5log10 lower than the RNeasy Plant mini kit. Nucleic acid was extracted from 19 grapevine-leaf samples with SMPs and the two commercial kits and subsequently screened for HSVd and GYSVd-1 by RT-qPCR. Regardless of HSVd or GYSVd-1, SMPs method outperforms other methods on both positive rate and the viroid load. In conclusion, SMPs method was able to efficiently extract the nucleic acid of RNA viruses or viroids, especially grapevine viroids, from lily-leaf or grapevine-leaf samples for RT-qPCR detection. Copyright © 2013 Elsevier B.V. All rights reserved.

Quantification of active principles and pigments in leaf extracts of Isatis tinctoria by HPLC/UV/MS.

PubMed

Mohn, Tobias; Potterat, Olivier; Hamburger, Matthias

2007-02-01

An HPLC method has been developed and validated for the quantification of the pharmacologically active principles tryptanthrin (1), 1,3-dihydro-3-[(4-hydroxy-3,5-dimethoxyphenyl)methylene]-2 H-indol-2-one (indolinone) (3), indirubin (4), alpha-linolenic acid (2), and indigo (5), an isomer of indirubin, in extracts from the traditional anti-inflammatory plant Isatis tinctoria (woad). The chromatographic separation was performed on a C-18 column with a linear gradient of acetonitrile in water containing 0.1% formic acid. The method combines UV and electrospray MS detection in the positive ion mode for the detection of the alkaloids, with a switch to the negative mode for the analysis of alpha-linolenic acid. The method was applied to the analysis of woad extracts obtained by supercritical fluid (SFE) CO2 extraction, and by pressurized liquid extraction (PLE) with dichloromethane and methanol, respectively. While the highest concentration of alpha-linolenic acid was found in the SFE extract (7.43%), the concentrations of tryptanthrin , indolinone, indirubin and indigo were the highest in the dichloromethane extract (0.30, 0.035, 2.48 and 0.84%, respectively). Compound 3 was not detected in the methanolic extract and only traces of compounds 1, 4 and 5 and low amount of alpha-linolenic acid (0.39%) were present in this extract.

Chemical Composition Analysis of Extracts from Ficus Hirta Using Supercritical Fluid

NASA Astrophysics Data System (ADS)

Deng, S. B.; Chen, J. P.; Chen, Y. Z.; Yu, C. Q.; Yang, Y.; Wu, S. H.; Chen, C. Z.

2018-05-01

Ficus hirta was extracted by supercritical carbon dioxide. The volatile chemical components of extracts were analyzed using gas chromatography-mass spectrometry (GC-MS). The percentage of products extracted by Supercritical Fluid Extraction(SFE) was 2.5%. Nineteen volatile compounds were identified. The main volatile components were Elemicin, Psoralen, Palmitic acid, Bergapten, α-Linolenic acid, Medicarpin, Retinoic Acid, Maackiain, and Squalene. The method is simple and quick, and can be used for the preliminary analysis of chemical constituents of supercritical extracts of Ficus hirta.

A novel method for harmless disposal and resource reutilization of steel wire rope sludges.

PubMed

Zhang, Li; Liu, Yang-Sheng

2016-10-01

Rapid development of steel wire rope industry has led to the generation of large quantities of pickling sludge, which causes significant ecological problems and considerable negative environmental effects. In this study, a novel method was proposed for harmless disposal and resource reutilization of the steel wire rope sludge. Based on the method, two steel wire rope sludges (the Pb sludge and the Zn sludge) were firstly extracted by hydrochloric or sulfuric acid and then mixed with the hydrochloride acid extracting solution of aluminum skimmings to produce composite polyaluminum ferric flocculants. The optimum conditions (acid concentration, w/v ratio, reaction time, and reaction temperature) for acid extraction of the sludges were studied. Results showed that 97.03 % of Pb sludge and 96.20 % of Zn sludge were extracted. Leaching potential of the residues after acid extraction was evaluated, and a proposed treatment for the residues had been instructed. The obtained flocculant products were used to purify the real domestic wastewater and showed an equivalent or better performance than the commercial ones. This method is environmental-friendly and cost-effective when compared with the conventional sludge treatments.

Method for forming an extraction agent for the separation of actinides from lanthanides

DOEpatents

Klaehn, John R.; Harrup, Mason K.; Law, Jack D.; Peterman, Dean R.

2010-04-27

An extraction agent for the separation of trivalent actinides from lanthanides in an acidic media and a method for forming same are described, and wherein the methodology produces a stable regiospecific and/or stereospecific dithiophosphinic acid that can operate in an acidic media having a pH of less than about 7.

Development of an improved sample preparation platform for acidic endogenous hormones in plant tissues using electromembrane extraction.

PubMed

Suh, Joon Hyuk; Han, Sang Beom; Wang, Yu

2018-02-02

Despite their importance in pivotal signaling pathways due to trace quantities and complex matrices, the analysis of plant hormones is a challenge. Here, to improve this issue, we present an electromembrane extraction technology combined with liquid chromatography-tandem mass spectrometry for determination of acidic plant hormones including jasmonic acid, abscisic acid, salicylic acid, benzoic acid, gibberellic acid and gibberellin A 4 in plant tissues. Factors influencing extraction efficiency, such as voltage, extraction time and stirring rate were optimized using a design of experiments. Analytical performance was evaluated in terms of specificity, linearity, limit of quantification, precision, accuracy, recovery and repeatability. The results showed good linearity (r 2  > 0.995), precision and acceptable accuracy. The limit of quantification ranged from 0.1 to 10 ng mL -1 , and the recoveries were 34.6-50.3%. The developed method was applied in citrus leaf samples, showing better clean-up efficiency, as well as higher sensitivity compared to a previous method using liquid-liquid extraction. Organic solvent consumption was minimized during the process, making it an appealing method. More noteworthy, electromembrane extraction has been scarcely applied to plant tissues, and this is the first time that major plant hormones were extracted using this technology, with high sensitivity and selectivity. Taken together, this work gives not only a novel sample preparation platform using an electric field for plant hormones, but also a good example of extracting complex plant tissues in a simple and effective way. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of silver, antimony, bismuth, copper, cadmium and indium in ores, concentrates and related materials by atomic-absorption spectrophotometry after methyl isobutyl ketone extraction as iodides.

PubMed

Donaldson, E M; Wang, M

1986-03-01

Methods for determining ~ 0.2 mug g or more of silver and cadmium, ~ 0.5 mug g or more of copper and ~ 5 mug g or more of antimony, bismuth and indium in ores, concentrates and related materials are described. After sample decomposition and recovery of antimony and bismuth retained by lead and calcium sulphates, by co-precipitation with hydrous ferric oxide at pH 6.20 +/- 0.05, iron(III) is reduced to iron(II) with ascorbic acid, and antimony, bismuth, copper, cadmium and indium are separated from the remaining matrix elements by a single methyl isobutyl ketone extraction of their iodides from ~2M sulphuric acid-0.1M potassium iodide. The extract is washed with a sulphuric acid-potassium iodide solution of the same composition to remove residual iron and co-extracted zinc, and the extracted elements are stripped from the extract with 20% v v nitric acid-20% v v hydrogen peroxide. Alternatively, after the removal of lead sulphate by filtration, silver, copper, cadmium and indium can be extracted under the same conditions and stripped with 40% v v nitric acid-25% v v hydrochloric acid. The strip solutions are treated with sulphuric and perchloric acids and ultimately evaporated to dry ness. The individual elements are determined in a 24% v v hydrochloric acid medium containing 1000 mug of potassium per ml by atomic-absorption spectrophotometry with an air-acetylene flame. Tin, arsenic and molybdenum are not co-extracted under the conditions above. Results obtained for silver, antimony, bismuth and indium in some Canadian certified reference materials by these methods are compared with those obtained earlier by previously published methods.

System and method for conditioning a hardwood pulp liquid hydrolysate

DOE Office of Scientific and Technical Information (OSTI.GOV)

Waite, Darrell; Arnold, Richard; St. Pierre, James

2015-06-30

A system and method for hardwood pulp liquid hydrolysate conditioning includes a first evaporator receives a hardwood mix extract and outputting a quantity of vapor and extract. A hydrolysis unit receives the extract, hydrolyzes and outputs to a lignin separation device, which separates and recovers a quantity of lignin. A neutralization device receives extract from the lignin separation device and a neutralizing agent, producing a mixture of solid precipitate and a fifth extract. The solid precipitate is removed from the fifth extract. A second evaporator removes a quantity of acid from the fifth extract in a vapor form. This vapormore » may be recycled to improve total acid recovery or discarded. A desalination device receives the diluted extract, separates out some of the acid and salt and outputs a desalinated solution.« less

Determination of caffeoylquinic acids in feed and related products by focused ultrasound solid-liquid extraction and ultra-high performance liquid chromatography-mass spectrometry.

PubMed

Tena, M T; Martínez-Moral, M P; Cardozo, P W

2015-06-26

A method to determine caffeoylquinic acids (CQAs) in three sources (herbal extract, feed additive and finished feed) using for the first time focused ultrasound solid-liquid extraction (FUSLE) followed by ultra-high performance liquid chromatography (UPLC) coupled to quadrupole-time of flight mass spectrometry is presented. Pressurized liquid extraction (PLE) was also tested as extraction technique but it was discarded because cynarin was not stable under temperature values used in PLE. The separation of the CQAs isomers was carried out in only seven minutes. FUSLE variables such as extraction solvent, power and time were optimized by a central composite design. Under optimal conditions, FUSLE extraction was performed with 8mL of an 83:17 methanol-water mixture for 30s at a power of 60%. Only two extraction steps were found necessary to recover analytes quantitatively. Sensitivity, linearity, accuracy and precision were established. Matrix effect was studied for each type of sample. It was not detected for mono-CQAs, whereas the cynarin signal was strongly decreased due to ionization suppression in presence of matrix components; so the quantification by standard addition was mandatory for the determination of di-caffeoylquinic acids. Finally, the method was applied to the analysis of herbal extracts, feed additives and finished feed. In all samples, chlorogenic acid was the predominant CQA, followed by criptochlorogenic acid, neochlorogenic acid and cynarin. The method allows an efficient determination of chlorogenic acid with good recovery rates. Therefore, it may be used for screening of raw material and for process and quality control in feed manufacture. Copyright © 2015 Elsevier B.V. All rights reserved.

Ultrasound-assisted extraction of amino acids from grapes.

PubMed

Carrera, Ceferino; Ruiz-Rodríguez, Ana; Palma, Miguel; Barroso, Carmelo G

2015-01-01

Recent cultivar techniques on vineyards can have a marked influence on the final nitrogen content of grapes, specifically individual amino acid contents. Furthermore, individual amino acid contents in grapes are related to the final aromatic composition of wines. A new ultrasound-assisted method for the extraction of amino acids from grapes has been developed. Several extraction variables, including solvent (water/ethanol mixtures), solvent pH (2-7), temperature (10-70°C), ultrasonic power (20-70%) and ultrasonic frequency (0.2-1.0s(-)(1)), were optimized to guarantee full recovery of the amino acids from grapes. An experimental design was employed to optimize the extraction parameters. The surface response methodology was used to evaluate the effects of the extraction variables. The analytical properties of the new method were established, including limit of detection (average value 1.4mmolkg(-)(1)), limit of quantification (average value 2.6mmolkg(-)(1)), repeatability (average RSD=12.9%) and reproducibility (average RSD=15.7%). Finally, the new method was applied to three cultivars of white grape throughout the ripening period. Copyright © 2014 Elsevier B.V. All rights reserved.

A simple one-step ultrasonic-assisted extraction and derivatization method coupling to high-performance liquid chromatographyfor the determination of ε-aminocaproic acid and amino acids in cosmetics.

PubMed

Du, Yuanqi; Xia, Ling; Xiao, Xiaohua; Li, Gongke; Chen, Xiaoguang

2018-06-15

Nowadays, the safety of cosmetics is a widespread concern. Amines are common cosmetic additives. Some of them such as amino acids are beneficial. Another kind of amines, however, ε-aminocaproic acid (EACA) is prohibited to add into cosmetics for its adverse reactions. In this study, a simple, rapid, sensitive and eco-friendly one-step ultrasonic-assisted extraction and derivatization (UAE-D) method was developed for determination of EACA and amino acids in cosmetics by coupling with high-performance liquid chromatography (HPLC). By using this sample preparation method, extraction and derivatization of EACA and amino acids were finished in one step in ultrasound field. During this procedure, 4-fluoro-7-nitrobenzofurazan (NBD-F)was applied as derivatization reagent. The extraction conditions including the amount of NBD-F, extraction and derivatization temperature, the ultrasonic vibration time and pH value of the aqueous phase were evaluated. Meanwhile, the extraction mechanism was investigated. Under optimized conditions, the method detection limits were 0.086-0.15 μg/L, and method quantitation limits were 0.29-0.47 μg/L with RSDs less than 3.7% (n = 3). The recoveries of EACA and amino acids obtained from cosmetic samples were in range from 76.9% to 122.3%. Amino acids were found in all selected samples and quantified in range from 1.9 ± 0.9 to 677.2 ± 17.9 μg/kg. And EACA was found and quantified with the contents of 1284.3 ± 22.1 μg/kg in a toner sample. This UAE-D-HPLC method shortened and simplified the sample pretreatment as well as enhanced the sensitivity of analytical method. In our record, only 10 min was needed for the total sample preparation process. And the method detection limits were two orders of magnitude less than literature reports. Furthermore, we reduced the consumption of solvent and minimized the usage of organic solvents, which made our method moving towards green analytical chemistry. In brief, our UAE-D-HPLC method is a simple, rapid, sensitive and eco-friendly analytical method for the determination of EACA and amino acids in cosmetics. Copyright © 2018 Elsevier B.V. All rights reserved.

Ionic liquids based microwave-assisted extraction of lichen compounds with quantitative spectrophotodensitometry analysis.

PubMed

Bonny, Sarah; Paquin, Ludovic; Carrié, Daniel; Boustie, Joël; Tomasi, Sophie

2011-11-30

Ionic liquids based extraction method has been applied to the effective extraction of norstictic acid, a common depsidone isolated from Pertusaria pseudocorallina, a crustose lichen. Five 1-alkyl-3-methylimidazolium ionic liquids (ILs) differing in composition of alkyl chain and anion were investigated for extraction efficiency. The extraction amount of norstictic acid was determined after recovery on HPTLC with a spectrophotodensitometer. The proposed approaches (IL-MAE and IL-heat extraction (IL-HE)) have been evaluated in comparison with usual solvents such as tetrahydrofuran in heat-reflux extraction and microwave-assisted extraction (MAE). The results indicated that both the characteristics of the alkyl chain and anion influenced the extraction of polyphenolic compounds. The sulfate-based ILs [C(1)mim][MSO(4)] and [C(2)mim][ESO(4)] presented the best extraction efficiency of norstictic acid. The reduction of the extraction times between HE and MAE (2 h-5 min) and a non-negligible ratio of norstictic acid in total extract (28%) supports the suitability of the proposed method. This approach was successfully applied to obtain additional compounds from other crustose lichens (Pertusaria amara and Ochrolechia parella). Copyright © 2011 Elsevier B.V. All rights reserved.

Depuration Study of Heavy Metal Lead (Pb) and Copper (Cu) in Green Mussels Perna viridis through Continues-discontinues and Acid Extraction Methods

NASA Astrophysics Data System (ADS)

Budiawan; Bakri, Ridla; Cahaya Dani, Intan; Handayani, Sri; Ade Kurnia Putri, Rizki; Tamala, Riska

2018-01-01

Green mussel or Perna viridis is filter feeder, which is very susceptible to heavy metals. It takes an effort to release heavy metal contents on the green shell, one of method that can be used to release heavy metal from green shell is depuration proccess. In this research, the depuration process was conducted by continues method of depuration, discontinues method by using various kind of water and acid extraction. The optimum time of continues depuration method is 1.5 hours, with circulation speed 250 L/h and result of Pb metal content decreased is equal to 30.048% and 29.748% for Cu. In the discontinues method, the optimum result was reached at 100oC by using PAM water as the media at 3 h immersion period with decrease of Pb metal content 35.001% and Cu metal content 39.015%. In the acid extraction method, the optimum condition was achieved by 11% acetic acid solvent with decreasing of Pb and Cu levels are 88.224% and 76.298%. For the determination of protein content, the decrease of protein content obtained by treatment with 11% acetic acid extract showed decrease of protein content 36.656% with Kjeldahl method.

[Determination of three phenoxyalkanoic acid herbicides in blood using gas chromatography coupled with solid-phase extraction and derivatization].

PubMed

Xin, Guobin; Tan, Jiayi; Yao, Lijuan; Zhu, Yu; Jiang, Zhaolin; Song, Hui

2008-01-01

A method for the determination of three phenoxyalkanoic acid herbicides, 2,4-dichlorophenoxyacetic acid (2,4-D), 2-(2,4-dichlorophenoxy)-propanoic acid (2,4-DP), and 4-chloro-2-methylphenoxy-acetic acid (MCPA), in blood was developed. The blood sample was diluted with 0.1 mol/L hydrochloric acid, and extracted by solid-phase extraction using porous resin GDX401 as adsorbent and ethyl ether as eluent. The extract was esterified with dichloropropanol in the presence of sulfuric acid as catalyst. The derivatives were analysed by gas chromatography with electron-capture detection. The detection limits of 2,4-D, 2,4-DP and MCPA were 20, 8 and 40 ng/mL, respectively. In quantitative analysis, 2,4-dichlorophenylacetic acid was used as an internal standard. The linear relationships and recoveries were satisfactory. The derivatization of the three herbicides with methanol, ethanol, n-propanol, n-butanol, and trifluoroethanol were also studied, and the analytical methods of these derivatization were compared with that of dichloropropanol as esterifying agent. The method is sensitive enough for the examination of the poison samples in actual.

Health Risk Assessment of Lead Ingestion Exposure by Particle Sizes in Crumb Rubber on Artificial Turf Considering Bioavailability

PubMed Central

Kim, Sunduk; Yang, Ji-Yeon; Kim, Ho-Hyun; Yeo, In-Young; Shin, Dong-Chun

2012-01-01

Objectives The purpose of this study was to assess the risk of ingestion exposure of lead by particle sizes of crumb rubber in artificial turf filling material with consideration of bioavailability. Methods This study estimated the ingestion exposure by particle sizes (more than 250 um or less than 250 um) focusing on recyclable ethylene propylene diene monomer crumb rubber being used as artificial turf filling. Analysis on crumb rubber was conducted using body ingestion exposure estimate method in which total content test method, acid extraction method and digestion extraction method are reflected. Bioavailability which is a calibrating factor was reflected in ingestion exposure estimate method and applied in exposure assessment and risk assessment. Two methods using acid extraction and digestion extraction concentration were compared and evaluated. Results As a result of the ingestion exposure of crumb rubber material, the average lead exposure amount to the digestion extraction result among crumb rubber was calculated to be 1.56×10-4 mg/kg-day for low grade elementary school students and 4.87×10-5 mg/kg-day for middle and high school students in 250 um or less particle size, and that to the acid extraction result was higher than the digestion extraction result. Results of digestion extraction and acid extraction showed that the hazard quotient was estimated by about over 2 times more in particle size of lower than 250 um than in higher than 250 um. There was a case of an elementary school student in which the hazard quotient exceeded 0.1. Conclusions Results of this study confirm that the exposure of lead ingestion and risk level increases as the particle size of crumb rubber gets smaller. PMID:22355803

Pharmacological activities of the organic extracts and fatty acid composition of the petroleum ether extract from Haplophyllum tuberculatum leaves.

PubMed

Hamdi, Assia; Majouli, Kaouther; Abdelhamid, Amal; Marzouk, Belsem; Belghith, Hèla; Chraief, Imed; Bouraoui, Abderrahman; Marzouk, Zohra; Heyden, Yvan Vander

2018-04-24

Haplophyllum tuberculatum is used in traditional medicine to treat many disorders including inflammation and pain. The aim of this study is to investigate the organic extracts from H. tuberculatum leaves against inflammation, gastric ulcer and pain. Acute toxicity was studied in vivo to determine the toxic doses of the organic extracts. Anti-inflammatory activity was also evaluated in vivo using carrageenan-induced paw edema in Wistar rats. Gastroprotective activity was tested using the HCl/ethanol-induced gastric ulcer test in rats. Peripheral and central analgesic activities were assessed using the acetic acid-induced writhing test and the hot-plate method, respectively. The chemical composition of the fatty acids in the petroleum ether (PE) extract was determined with GC-MS. At 25, 50 and 100mg/kg PE extract was the most active against inflammation. Percentages inhibition 5h after carrageenan-injection were 51.12; 86.71% and 96.92%, respectively. The same extract at 100mg/kg showed good analgesic activities using the acetic acid-induced writhing test and the hot-plate method. The chloroform, ethyl acetate (EtOAc) and butanolic (n-BuOH) extracts exhibited strong anti-inflammatory, gastroprotective and analgesic activities at 100mg/kg. The GC-FID analysis revealed that the PE extract was rich in γ-linolenic acid (45.50%) followed by palmitic acid (18.48%), linoleic acid (10.73%), erucic acid (4.72), stearic acid (3.96%) and oleic acid (2.57%). The results of the present study support the traditional use of the leaves of H. tuberculatum and may possibly serve as prospective material for further development of safe new phytochemical anti-inflammatory, gastroprotective and/or analgesic agents. Copyright © 2018 Elsevier B.V. All rights reserved.

Separation and quantitation of three acidic herbicide residues in tobacco and soil by dispersive solid-phase extraction and UPLC-MS/MS.

PubMed

Xiong, Wei; Tao, Xiaoqiu; Pang, Su; Yang, Xue; Tang, GangLing; Bian, Zhaoyang

2014-01-01

A method for the determination of three acidic herbicides, dicamba, 2,4-dichlorophenoxyacetic acid (2,4-D) and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T) in tobacco and soil has been developed based on the use of liquid-liquid extraction and dispersive solid-phase extraction (dispersive-SPE) followed by UPLC-MS/MS. Two percentage of (v/v) formic acid in acetonitrile as the extraction helped partitioning of analytes into the acetonitrile phase. The extract was then cleaned up by dispersive-SPE using primary secondary amine as selective sorbents. Quantitative analysis was done in the multiple-reaction monitoring mode using stable isotope-labeled internal standards for each compound. A separate internal standard for each analyte is required to minimize sample matrix effects on each analyte, which can lead to poor analyte recoveries and decreases in method accuracy and precision. The total analysis time was <4 min. The linear range of the method was from 1 to 100 ng mL(-1) with a limit of detection of each herbicide varied from 0.012 to 0.126 ng g(-1). The proposed method is faster, more sensitive and selective than the traditional methods and more accurate and robust than the published LC-MS/MS methods. © The Author [2013]. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

[AAPH scavenging activities of 22 flavonoids and phenolic acids and 9 extracts of Chinese materia medica].

PubMed

Dai, Huiqing; Chen, Chengyu; Yang, Bin

2010-09-01

To investigate the AAPH scavenging activities of 22 flavonoids and phenolic acids and 9 extracts of Chinese materia medica. The antioxidant activities of the samples were evaluated by an oxygen radical absorbance capacity method (ORAC), at the same time, the total contents of flavonoids and phenolic the 9 herb extracts were analyzed by Folin-Ciocalteu method, and the active components were qualitatively and quantitatively analyzed by an HPLC method. It was found that the tea extract showed the strongest AAPH activity with the ORAC value of 4786.40 micromol x g(-1) whereas safflower demonstrated the weakest activity with the ORAC value of 784.04 micromol x g(-1). As for compounds, quercetin had the strongest AAPH activity with the ORAC value of 12.90 while ( - )-EGC had the weakest activity with the ORAC value of 2.47. A quantitative relationship was obtained to describe the AAPH scavenging activity of the herb extracts: Y = 1844.8 lnX-3577.5, r = 0.8675, where Y stands for the ORAC vaule, and X stands for the concentration of total phenolic acids. Flavonoids and phenolic acids are the AAPH scavenging active ingredients in the Chinese herb extracts. It's a good way to study the antioxidant activity of Chinese herb extract and its chemical composition by combing ORAC method and HPLC method.

Quantitative determination of plant phenolics in Urtica dioica extracts by high-performance liquid chromatography coupled with tandem mass spectrometric detection.

PubMed

Orčić, Dejan; Francišković, Marina; Bekvalac, Kristina; Svirčev, Emilija; Beara, Ivana; Lesjak, Marija; Mimica-Dukić, Neda

2014-01-15

A method for quantification of 45 plant phenolics (including benzoic acids, cinnamic acids, flavonoid aglycones, C- and O-glycosides, coumarins, and lignans) in plant extracts was developed, based on reversed phase HPLC separation of extract components, followed by tandem mass spectrometric detection. The phenolic profile of 80% MeOH extracts of the stinging nettle (Urtica dioica L.) herb, root, stem, leaf and inflorescence was obtained by using this method. Twenty-one of the investigated compounds were present at levels above the reliable quantification limit, with 5-O-caffeoylquinic acid, rutin and isoquercitrin as the most abundant. The inflorescence extracts were by far the richest in phenolics, with the investigated compounds amounting 2.5-5.1% by weight. As opposed to this, the root extracts were poor in phenolics, with only several acids and derivatives being present in significant amounts. The results obtained by the developed method represent the most detailed U. dioica chemical profile so far. Copyright © 2013 Elsevier Ltd. All rights reserved.

Solid Phase Micro-extraction (SPME) with In Situ Transesterification: An Easy Method for the Detection of Non-volatile Fatty Acid Derivatives on the Insect Cuticle.

PubMed

Kühbandner, Stephan; Ruther, Joachim

2015-06-01

Triacylglycerides (TAGs) and other non-volatile fatty acid derivatives (NFADs) occur in large amounts in the internal tissues of insects, but their presence on the insect cuticle is controversially discussed. Most studies investigating cuticular lipids of insects involve solvent extraction, which implies the risk of extracting lipids from internal tissues. Here, we present a new method that overcomes this problem. The method employs solid phase micro-extraction (SPME) to sample NFADs by rubbing the SPME fiber over the insect cuticle. Subsequently, the sampled NFADs are transesterified in situ with trimethyl sulfonium hydroxide (TMSH) into more volatile fatty acid methyl esters (FAMEs), which can be analyzed by standard GC/MS. We performed two types of control experiments to enable significant conclusions: (1) to rule out contamination of the GC/MS system with NFADs, and (2) to exclude the presence of free fatty acids on the insect cuticle, which would also furnish FAMEs after TMSH treatment, and thus might simulate the presence of NFADs. In combination with these two essential control experiments, the described SPME technique can be used to detect TAGs and/or other NFADs on the insect cuticle. We analyzed six insect species from four insect orders with our method and compared the results with conventional solvent extraction followed by ex situ transesterification. Several fatty acids typically found as constituents of TAGs were detected by the SPME method on the cuticle of all species analyzed. A comparison of the two methods revealed differences in the fatty acid compositions of the samples. Saturated fatty acids showed by trend higher relative abundances when sampled with the SPME method, while several minor FAMEs were detected only in the solvent extracts. Our study suggests that TAGs and maybe other NFADs are far more common on the insect cuticle than usually thought.

Fatty acid profile and elemental content of avocado (Persea americana Mill.) oil--effect of extraction methods.

PubMed

Reddy, Mageshni; Moodley, Roshila; Jonnalagadda, Sreekanth B

2012-01-01

Interest in vegetable oil extracted from idioblast cells of avocado fruit is growing. In this study, five extraction methods to produce avocado oil have been compared: traditional solvent extraction using a Soxhlet or ultrasound, Soxhlet extraction combined with microwave or ultra-turrax treatment and supercritical fluid extraction (SFE). Traditional Soxhlet extraction produced the most reproducible results, 64.76 ± 0.24 g oil/100 g dry weight (DW) and 63.67 ± 0.20 g oil/100 g DW for Hass and Fuerte varieties, respectively. Microwave extraction gave the highest yield of oil (69.94%) from the Hass variety. Oils from microwave extraction had the highest fatty acid content; oils from SFE had wider range of fatty acids. Oils from Fuerte variety had a higher monounsaturated: saturated FA ratio (3.45-3.70). SFE and microwave extraction produced the best quality oil, better than traditional Soxhlet extraction, with the least amount of oxidizing metals present. Copyright © Taylor & Francis Group, LLC

An efficient method for extraction of astaxanthin from green alga Haematococcus pluvialis.

PubMed

Sarada, R; Vidhyavathi, R; Usha, D; Ravishankar, G A

2006-10-04

Haematococcus pluvialis is one of the potent organisms for production of astaxanthin, a high value ketocarotenoid. Astaxanthin is accumulated in thick-walled cyst cells of Haematococcus. The thick cell wall is made up of sporopollenin-like material, algaenan, which hinders solvent extraction of astaxanthin. In the present study, an improved method for extraction of astaxanthin without homogenization of cells is reported. Extractability of astaxanthin from cyst cells was evaluated by treating cells with various solvents and pretreating the cells with organic and mineral acids at 70 degrees C followed by acetone extraction. Hydrochloric acid treatment facilitated 86-94% extractability of astaxanthin. Treatment time, temperature, and concentration of the acid were found to be critical factors for maximum extractability. The treatment did not affect the astaxanthin ester profile and the treated cells can be preserved until further use.

Comparison of manual and automated nucleic acid extraction methods from clinical specimens for microbial diagnosis purposes.

PubMed

Wozniak, Aniela; Geoffroy, Enrique; Miranda, Carolina; Castillo, Claudia; Sanhueza, Francia; García, Patricia

2016-11-01

The choice of nucleic acids (NAs) extraction method for molecular diagnosis in microbiology is of major importance because of the low microbial load, different nature of microorganisms, and clinical specimens. The NA yield of different extraction methods has been mostly studied using spiked samples. However, information from real human clinical specimens is scarce. The purpose of this study was to compare the performance of a manual low-cost extraction method (Qiagen kit or salting-out extraction method) with the automated high-cost MagNAPure Compact method. According to cycle threshold values for different pathogens, MagNAPure is as efficient as Qiagen for NA extraction from noncomplex clinical specimens (nasopharyngeal swab, skin swab, plasma, respiratory specimens). In contrast, according to cycle threshold values for RNAseP, MagNAPure method may not be an appropriate method for NA extraction from blood. We believe that MagNAPure versatility reduced risk of cross-contamination and reduced hands-on time compensates its high cost. Copyright © 2016 Elsevier Inc. All rights reserved.

Quality control of herbs: determination of amino acids in Althaea officinalis, Matricaria chamomilla and Taraxacum officinale.

PubMed

Qureshi, Muhammad Nasimullah; Stecher, Guenther; Bonn, Guenther Karl

2014-05-01

Analysis of raw materials and final products need reliable methods for the standardization of natural product drugs. Legal guideline also emphasizes on the qualitative and quantitative analyses of the plant constituents in an herbal product. In this study, thin layer chromatography (TLC) and amino acid analyzer was used for the determination of amino acids in plant extracts. Samples for this study were standards and aqueous extracts from Althaea officinalis, Matricaria chamomilla and Taraxacum officinale. Different amino acids in the extracts were detected through TLC. An automatic amino acid analyzer was used for the quantification of amino acids in the plant extracts under study.

Comparison of different extraction methods and HPLC quantification of prenylated and unprenylated phenylpropanoids in raw Italian propolis.

PubMed

Taddeo, Vito Alessandro; Epifano, Francesco; Fiorito, Serena; Genovese, Salvatore

2016-09-10

In this paper the presence of selected prenylated and unprenylated phenylpropanoids, namely ferulic acid 1, boropinic acid 2, 4'-geranyloxyferulic acid 3, umbelliferone 4, 7-isopentenyloxycoumarin 5, and auraptene 6, have been determined in Italian raw propolis after having been extracted with different methodologies. An aqueous solution of β-cyclodextrin was the best extraction method for ferulic acid 1, treatment with indifferently EtOH or aqueous β-cyclodextrin were the most effective one for umbelliferone 4, boropinic acid 2 gave the best yields either with H2O/β-cyclodextrin or olive oil treatment or in biphasic systems, maceration with biphasic mixtures of aqueous β-cyclodextrin and olive oil was seen to be the most effective procedure for 7-isopentenyloxycoumarin 5, the only method providing significant quantities of 4'-geranyloxyferulic acid 3 was the maceration of raw propolis with olive oil, and finally auraptene 4 was best extracted with absolute EtOH. "Classic" maceration in general performed better than ultrasound-assisted one. Copyright © 2016 Elsevier B.V. All rights reserved.

SEPARATION OF THORIUM FROM URANIUM BY EXTRACTION

DOEpatents

Bohlmann, E.G.

1959-07-28

A method is presented for the recovery and separation of uranium and thorium values contained in an aqueous nitric acid solution which is more than 3 M in nitric acid. The uranium and thorium containing solution preferable about 7 M in nitric acid is contacted with tributyl phosphatekerosene mixture. Both U and Th are extracted by the immiscible organic. After phase separation the Th is selectively back extracted by contacting with an aqueous nitric acid solution preferably between 0.1 to 1.5 M in nitric acid. The uranium which is still in the organic extractant phase may be recovered by contacting with water.

The Effect of Two Methods of Pomegranate (Punica granatum L) Juice Extraction on Quality During Storage at 4°C

PubMed Central

Antunes, Dulce

2004-01-01

The effect of two extraction methods of pomegranate juice on its quality and stability was evaluated. The first method consisted of separation of the seeds from fruits and centrifugation. The second method consisted of squeezing fruit halves with an electric lemon squeezer. During a period of 72 hours of cold storage at 4°C, the juices were evaluated for the presence of sugars, organic acids, and anthocyanins. Delphinidin 3-glucoside was identified to be the major anthocyanin present at the level of 45–69 mg/L. Among the organic acids, oxalic and tartaric acids dominated. The major sugars detected in pomegranate juice were glucose and sucrose. No significant differences in the content of sugars, organic acids, or anthocyanins in juices obtained through application of the two different extraction methods were detected, with the exception of the drastic decrease of cyanidin 3,5-diglucoside level in juice obtained by seed centrifugation. The pH did not show differences between treatments. Titrable acidity and the level of sugars expressed as °Brix decreased after 32 and 15 hours after extraction, respectively, when juice was obtained by centrifuging the seeds. PMID:15577198

The Effect of Two Methods of Pomegranate (Punica granatum L) Juice Extraction on Quality During Storage at $4^\\circ$ C.

PubMed

Miguel, Graça; Dandlen, Susana; Antunes, Dulce; Neves, Alcinda; Martins, Denise

2004-01-01

The effect of two extraction methods of pomegranate juice on its quality and stability was evaluated. The first method consisted of separation of the seeds from fruits and centrifugation. The second method consisted of squeezing fruit halves with an electric lemon squeezer. During a period of 72 hours of cold storage at $4^\\circ$ C, the juices were evaluated for the presence of sugars, organic acids, and anthocyanins. Delphinidin 3-glucoside was identified to be the major anthocyanin present at the level of 45-69 mg/L. Among the organic acids, oxalic and tartaric acids dominated. The major sugars detected in pomegranate juice were glucose and sucrose. No significant differences in the content of sugars, organic acids, or anthocyanins in juices obtained through application of the two different extraction methods were detected, with the exception of the drastic decrease of cyanidin $3,5$ -diglucoside level in juice obtained by seed centrifugation. The pH did not show differences between treatments. Titrable acidity and the level of sugars expressed as ${}^{\\circ}$ Brix decreased after 32 and 15 hours after extraction, respectively, when juice was obtained by centrifuging the seeds.

Method for extracting lanthanides and actinides from acid solutions by modification of Purex solvent

DOEpatents

Horwitz, E.P.; Kalina, D.G.

1984-05-21

A process has been developed for the extraction of multivalent lanthanide and actinide values from acidic waste solutions, and for the separation of these values from fission product and other values, which utilizes a new series of neutral bi-functional extractants, the alkyl(phenyl)-N, N-dialkylcarbamoylmethylphosphine oxides, in combination with a phase modifier to form an extraction solution. The addition of the extractant to the Purex process extractant, tri-n-butylphosphate in normal paraffin hydrocarbon diluent, will permit the extraction of multivalent lanthanide and actinide values from 0.1 to 12.0 molar acid solutions.

Analysis of mixtures of fatty acids and fatty alcohols in fermentation broth.

PubMed

Liu, Yilan; Chen, Ting; Yang, Maohua; Wang, Caixia; Huo, Weiyan; Yan, Daojiang; Chen, Jinjin; Zhou, Jiemin; Xing, Jianmin

2014-01-03

Microbial production of fatty acids and fatty alcohols has attracted increasing concerns because of energy crisis and environmental impact of fossil fuels. Therefore, simple and efficient methods for the extraction and quantification of these compounds become necessary. In this study, a high-performance liquid chromatography-refractive index detection (HPLC-RID) method was developed for the simultaneous quantification of fatty acids and fatty alcohols in these samples. The optimum chromatographic conditions are C18 column eluted with methanol:water:acetic acid (90:9.9:0.1, v/v/v); column temperature, 26°C; flow rate, 1.0mL/min. Calibration curves of all selected analytes showed good linearity (r(2)≥0.9989). The intra-day and inter-day relative standard deviations (RSDs) of the 10 compounds were less than 4.46% and 5.38%, respectively, which indicated that the method had good repeatability and precision. Besides, a method for simultaneous extraction of fatty acids and fatty alcohols from fermentation broth was optimized by orthogonal design. The optimal extraction conditions were as follows: solvent, ethyl acetate; solvent to sample ratio, 0.5:1; rotation speed, 2min at 260rpm; extraction temperature, 10°C. This study provides simple and fast methods to simultaneously extract and quantify fatty acids and fatty alcohols for the first time. It will be useful for the study of microbial production of these products. Copyright © 2013 Elsevier B.V. All rights reserved.

Physicochemical and Antioxidant Properties of Rice Bran Oils Produced from Colored Rice Using Different Extraction Methods.

PubMed

Mingyai, Sukanya; Kettawan, Aikkarach; Srikaeo, Khongsak; Singanusong, Riantong

2017-06-01

This study investigated the physicochemical and antioxidant properties of rice bran oil (RBO) produced from the bran of three rice varities; Khao Dawk Mali 105 (white rice), Red Jasmine rice (red rice) and Hom-nin rice (black rice) using three extraction methods including cold-press extraction (CPE), solvent extraction (SE) and supercritical CO 2 extraction (SC-CO 2 ). Yields, color, acid value (AV), free fatty acid (FFA), peroxide value (PV), iodine value (IV), total phenolic compound (TPC), γ-oryzanol, α-tocopherol and fatty acid profile were analyzed. It was found that the yields obtained from SE, SC-CO 2 and CPE extractions were 17.35-20.19%, 14.76-18.16% and 3.22-6.22%, respectively. The RBO from the bran of red and black rice samples exhibited high antioxidant activities. They also contained higher amount of γ-oryzanol and α-tocopherol than those of white rice sample. In terms of extraction methods, SC-CO 2 provided better qualities of RBO as evidenced by their physicochemical and antioxidant properties. This study found that RBO produced from the bran of black rice samples using SC-CO 2 extraction method showed the best physicochemical and antioxidant properties.

Recovery of Oil with Unsaturated Fatty Acids and Polyphenols from Chaenomelessinensis (Thouin) Koehne: Process Optimization of Pilot-Scale Subcritical Fluid Assisted Extraction.

PubMed

Zhu, Zhenzhou; Zhang, Rui; Zhan, Shaoying; He, Jingren; Barba, Francisco J; Cravotto, Giancarlo; Wu, Weizhong; Li, Shuyi

2017-10-22

The potential effects of three modern extraction technologies (cold-pressing, microwaves and subcritical fluids) on the recovery of oil from Chaenomelessinensis (Thouin) Koehne seeds have been evaluated and compared to those of conventional chemical extraction methods (Soxhlet extraction). This oil contains unsaturated fatty acids and polyphenols. Subcritical fluid extraction (SbFE) provided the highest yield-25.79 g oil/100 g dry seeds-of the three methods. Moreover, the fatty acid composition in the oil samples was analysed using gas chromatography-mass spectrometry. This analysis showed that the percentages of monounsaturated (46.61%), and polyunsaturated fatty acids (42.14%), after applying SbFE were higher than those obtained by Soxhlet, cold-pressing or microwave-assisted extraction. In addition, the oil obtained under optimized SbFE conditions (35 min extraction at 35 °C with four extraction cycles), showed significant polyphenol (527.36 mg GAE/kg oil), and flavonoid (15.32 mg RE/kg oil), content, had a good appearance and was of high quality.

Comparison of Oil Content and Fatty Acids Profile of Western Schley, Wichita, and Native Pecan Nuts Cultured in Chihuahua, Mexico.

PubMed

Rivera-Rangel, L R; Aguilera-Campos, K I; García-Triana, A; Ayala-Soto, J G; Chavez-Flores, D; Hernández-Ochoa, L

2018-01-01

Two different extraction processes, Soxhlet and ultrasound, were used to obtain the oil extracts of Western Schley, Wichita, and Native pecan nuts cultured in Chihuahua, Mexico. The aspects evaluated in this study were the extraction yield of the processes and fatty acids' profile of the resulting extracts. Gas chromatography coupled with mass spectrometry (GC-MS) was used to identify and determine the composition percentage of fatty acids present in pecan nuts oils extracted. The results obtained show that higher oil extraction yields were obtained by Soxhlet method with hexane (69.90%) in Wichita varieties. Wichita, Western Schley, and Native pecan nuts from Chihuahua are rich in PUFA (polyunsaturated fatty acids) and MUFA (monounsaturated fatty acids) and have low levels of SFA (saturated fatty acids). The predominant fatty acid present in all pecan nuts oils was linoleic acid followed by oleic acid. Myristic acid, palmitic acid, and linolenic acid were also identified in representative quantities. The results from this study suggest that there are statistically significant differences in the chemical composition of the pecan nuts oils extracted from the varieties cultured in Chihuahua, Mexico, and those cultivated in other regions of the world.

Comparison of Oil Content and Fatty Acids Profile of Western Schley, Wichita, and Native Pecan Nuts Cultured in Chihuahua, Mexico

PubMed Central

Rivera-Rangel, L. R.; Aguilera-Campos, K. I.; García-Triana, A.; Ayala-Soto, J. G.; Chavez-Flores, D.

2018-01-01

Two different extraction processes, Soxhlet and ultrasound, were used to obtain the oil extracts of Western Schley, Wichita, and Native pecan nuts cultured in Chihuahua, Mexico. The aspects evaluated in this study were the extraction yield of the processes and fatty acids' profile of the resulting extracts. Gas chromatography coupled with mass spectrometry (GC-MS) was used to identify and determine the composition percentage of fatty acids present in pecan nuts oils extracted. The results obtained show that higher oil extraction yields were obtained by Soxhlet method with hexane (69.90%) in Wichita varieties. Wichita, Western Schley, and Native pecan nuts from Chihuahua are rich in PUFA (polyunsaturated fatty acids) and MUFA (monounsaturated fatty acids) and have low levels of SFA (saturated fatty acids). The predominant fatty acid present in all pecan nuts oils was linoleic acid followed by oleic acid. Myristic acid, palmitic acid, and linolenic acid were also identified in representative quantities. The results from this study suggest that there are statistically significant differences in the chemical composition of the pecan nuts oils extracted from the varieties cultured in Chihuahua, Mexico, and those cultivated in other regions of the world. PMID:29610686

Development of the extraction method for the simultaneous determination of butyl-, phenyl- and octyltin compounds in sewage sludge.

PubMed

Zuliani, Tea; Lespes, Gaetane; Milacic, Radmila; Scancar, Janez

2010-03-15

The toxicity and bioaccumulation of organotin compounds (OTCs) led to the development of sensitive and selective analytical methods for their determination. In the past much attention was assigned to the study of OTCs in biological samples, water and sediments, coming mostly from marine environment. Little information about OTCs pollution of terrestrial ecosystems is available. In order to optimise the extraction method for simultaneous determination of butyl-, phenyl- and octyltin compounds in sewage sludge five different extractants (tetramethylammonium hydroxide, HCl in methanol, glacial acetic acid, mixture of acetic acid and methanol (3:1), and mixture of acetic acid, methanol and water (1:1:1)), the presence or not of a complexing agent (tropolone), and the use of different modes of extraction (mechanical stirring, microwave and ultrasonic assisted extraction) were tested. Extracted OTCs were derivatised with sodium tetraethylborate and determined by gas chromatography coupled with mass spectrometer. Quantitative extraction of butyl-, phenyl- and octyltin compounds was obtained by the use of glacial acetic acid as extractant and mechanical stirring for 16h or sonication for 30 min. The limits of detection and quantification for OTCs investigated in sewage sludge were in the ng S ng(-1) range. Copyright (c) 2009 Elsevier B.V. All rights reserved.

Extraction of Total Nucleic Acids From Ticks for the Detection of Bacterial and Viral Pathogens

PubMed Central

Crowder, Chris D.; Rounds, Megan A.; Phillipson, Curtis A.; Picuri, John M.; Matthews, Heather E.; Halverson, Justina; Schutzer, Steven E.; Ecker, David J.; Eshoo, Mark W.

2010-01-01

Ticks harbor numerous bacterial, protozoal, and viral pathogens that can cause serious infections in humans and domestic animals. Active surveillance of the tick vector can provide insight into the frequency and distribution of important pathogens in the environment. Nucleic-acid based detection of tick-borne bacterial, protozoan, and viral pathogens requires the extraction of both DNA and RNA (total nucleic acids) from ticks. Traditional methods for nucleic acid extraction are limited to extraction of either DNA or the RNA from a sample. Here we present a simple bead-beating based protocol for extraction of DNA and RNA from a single tick and show detection of Borrelia burgdorferi and Powassan virus from individual, infected Ixodes scapularis ticks. We determined expected yields for total nucleic acids by this protocol for a variety of adult tick species. The method is applicable to a variety of arthropod vectors, including fleas and mosquitoes, and was partially automated on a liquid handling robot. PMID:20180313

Comparison of methods of extracting messenger Ribonucleic Acid from ejaculated Porcine (Sus Scrofa) Spermatozoa

USDA-ARS?s Scientific Manuscript database

H. D. Guthrie, G.R. Welch, and L. A. Blomberg. Comparison of Methods of Extracting Messenger Ribonucleic Acid from Ejaculated Porcine (Sus Scrofa) Spermatozoa. Biotechnology and Germplasm Laboratory, Agricultural Research Service U. S. Department of Agriculture, Beltsville, MD 20705 The purpos...

Ultrasonic Removal of Mucilage for Pressurized Liquid Extraction of Omega-3 Rich Oil from Chia Seeds (Salvia hispanica L.).

PubMed

Castejón, Natalia; Luna, Pilar; Señoráns, Francisco J

2017-03-29

Chia (Salvia hispanica L.) seeds contain an important amount of edible oil rich in omega-3 fatty acids. Fast and alternative extraction techniques based on polar solvents, such as ethanol or water, have become relevant for oil extraction in recent years. However, chia seeds also contain a large amount of soluble fiber or mucilage, which makes difficult an oil extraction process with polar solvents. For that reason, the aim of this study was to develop a gentle extraction method for mucilage in order to extract chia oil with polar solvents using pressurized liquids and compare with organic solvent extraction. The proposed mucilage extraction method, using an ultrasonic probe and only water, was optimized at mild conditions (50 °C and sonication 3 min) to guarantee the omega-3 oil quality. Chia oil extraction was performed using pressurized liquid extraction (PLE) with different solvents and their mixtures at five different extraction temperatures (60, 90, 120, 150, and 200 °C). Optimal PLE conditions were achieved with ethyl acetate or hexane at 90 °C in only 10 min of static extraction time (chia oil yield up to 30.93%). In addition, chia oils extracted with nonpolar and polar solvents by PLE were analyzed by gas chromatography-mass spectrometry (GC-MS) to evaluate fatty acid composition at different extraction conditions. Chia oil contained ∼65% of α-linolenic acid regardless of mucilage extraction method, solvent, or temperature used. Furthermore, tocopherols and tocotrienols were also analyzed by HPLC in the extracted chia oils. The mucilage removal allowed the subsequent extraction of the chia oil with polar or nonpolar solvents by PLE producing chia oil with the same fatty acid and tocopherol composition as traditional extraction.

Novel assay system for acidic Peptide:N-glycanase (aPNGase) activity in crude plant extract.

PubMed

Uemura, Ryota; Ogura, Mikako; Matsumaru, Chihiro; Akiyama, Tsuyoshi; Maeda, Megumi; Kimura, Yoshinobu

2018-04-15

Acidic peptide:N-glycanase (aPNGase) plays a pivotal role in plant glycoprotein turnover. For the construction of aPNGase-knockout or -overexpressing plants, a new method to detect the activity in crude plant extracts is required because endogenous peptidases present in the extract hamper enzyme assays using fluorescence-labeled N-glycopeptides as a substrate. In this study, we developed a new method for measuring aPNGase activity in crude extracts from plant materials.

Comparison of extraction methods for the analysis of natural dyes in historical textiles by high-performance liquid chromatography.

PubMed

Valianou, Lemonia; Karapanagiotis, Ioannis; Chryssoulakis, Yannis

2009-12-01

Different methods for the extraction of Dactylopius coccus Costa, Rubia tinctorum L., Isatis tinctoria L., Reseda luteola L., Curcuma longa L. and Cotinus coggygria Scop. from wool fibres are investigated using high-performance liquid chromatography with diode array detector (HPLC-DAD). The efficiencies of five extraction methods which include the use of HCl (widely used extraction method), citric acid, oxalic acid, TFA and a combination of HCOOH and EDTA are compared on the basis of the (a) number, (b) relative quantities, measured as HPLC peak areas and (c) signal-to-noise ratios (S/N) of the compounds extracted from the wool substrates. Flavonoid glycosides and curcuminoids contained in R. luteola L. and C. longa L., respectively, according to liquid chromatography with mass spectrometry (LC-MS) identifications, are not detected after treating the fibres with HCl. All the other milder methods are successful in extracting these compounds. Experiments are performed using HPLC-DAD to compare the HPLC peak areas and the S/N of the following extracted compounds: indigotin, indirubin, curcumin, demethoxycurcumin, bisdemethoxycurcumin, fisetin, sulfuretin, luteolin, luteolin-7-O-glucoside, apigenin, carminic acid, alizarin, puruprin and rubiadin. It is shown that the TFA method provides overall the best results as it gives elevated extraction yields except for fisetin, luteolin, apigenin and luteolin-7-O-glucoside and highest S/N except for fisetin and luteolin-7-O-glucoside. It is noteworthy that treatment of the fibres with the typical HCl extraction method results overall in very low S/N. The TFA method is selected for further studies, as follows. First, it is applied on silk dyed samples and compared with the HCl method. The same relative differences of the TFA and HCl methods observed for the wool dyed samples are reported for the silk dyed samples too, except for rubiadin, luteolin and apigenin. Thus, in most cases, the nature of the substrate (wool or silk) appears to have negligible effects on the relative difference of the two extraction methods. Second, the selected TFA method is applied to treat wool and silk historical samples extracted from textiles of the Mamluk period, resulting in the identification of several colouring compounds. In all extraction methods mentioned above, DMSO is used to dissolve the dyes, after acid treatment.

[Study on extraction of the total saponins of Chinese yam].

PubMed

Zhang, Min; Du, Lin; Huang, Gui-dong; Zhong, Xian-feng

2007-07-01

A method for the determination of total saponins of Chinese yam was established. The dioscin was used as a standard compound, the vanillin-perchloric acid as chromogenic agent and glacial acetic acid as solvent. The extraction technique of asponins from Chinese yam was studied by spectrometric method. Extracting temperature, extracting time, ethanol concentration and the ratio of raw material and water were selected as four factors to design the orthogonal test, and the optical condition of extraction was obtained. The results showed that the optical condition of extraction was as following: extracting temperature 60 degrees C, extracting time 6 h, ethanol concetration 80%, and the ratio of raw material and water 1:8.

[Comparison of MPure-12 Automatic Nucleic Acid Purification and Chelex-100 Method].

PubMed

Shen, X; Li, M; Wang, Y L; Chen, Y L; Lin, Y; Zhao, Z M; Que, T Z

2017-04-01

To explore the forensic application value of MPure-12 automatic nucleic acid purification （MPure-12 Method） for DNA extraction by extracting and typing DNA from bloodstains and various kinds of biological samples with different DNA contents. Nine types of biological samples, such as bloodstains, semen stains, and saliva were collected. DNA were extracted using MPure-12 method and Chelex-100 method, followed by PCR amplification and electrophoresis for obtaining STR-profiles. The samples such as hair root, chutty, butt, muscular tissue, saliva stain, bloodstain and semen stain were typed successfully by MPure-12 method. Partial alleles were lacked in the samples of saliva, and the genotyping of contact swabs was unsatisfactory. Additional, all of the bloodstains （20 μL, 15 μL, 10 μL, 5 μL, 1 μL） showed good typing results using Chelex-100 method. But the loss of alleles occurred in 1 μL blood volume by MPure-12 method. MPure-12 method is suitable for DNA extraction of a certain concentration blood samples．Chelex-100 method may be better for the extraction of trace blood samples．This instrument used in nucleic acid extraction has the advantages of simplicity of operator, rapidity, high extraction efficiency, high rate of reportable STR-profiles and lower man-made pollution. Copyright© by the Editorial Department of Journal of Forensic Medicine

Extraction of acidic degradation products of organophosphorus chemical warfare agents. Comparison between silica and mixed-mode strong anion-exchange cartridges.

PubMed

Kanaujia, Pankaj K; Pardasani, Deepak; Gupta, A K; Kumar, Rajesh; Srivastava, R K; Dubey, D K

2007-08-17

The analysis of alkyl alkylphosphonic acids (AAPAs) and alkylphosphonic acids (APAs), the hydrolyzed products of nerve agents, constitutes an important aspect for verifying the compliance to the Chemical weapons convention (CWC). This work devotes on the development of solid-phase extraction method using polymeric mixed-mode strong anion-exchange (Oasis MAX) cartridges for extraction of AAPAs and APAs from water. The extracted analytes were analyzed by GC-MS under full scan and selected ion monitoring mode. The extraction efficiencies of MAX and silica-based anion-exchange cartridges were compared, and results revealed that MAX sorbents yielded better recoveries. Extraction parameters, such as loading capacity, extraction solvent, its volume, and washing solvent were optimized. Best recoveries were obtained using 1 mL of acidic methanol (0.1 M), and limits of detection could be achieved up to 5 x 10(-4) microg mL(-1) (in SIM) and 0.05 microg mL(-1) in full scan mode. The method was successfully employed for the detection and identification of alkylphosphonic acids present in soil sample sent by the Organization for Prohibition of Chemical Weapons (OPCW) in the official proficiency tests.

Effects of Different Extraction Methods on the Extraction Rates of Five Chemical Ingredients of Swertia mussotii Franch by UPLC-ESI-MS/MS

NASA Astrophysics Data System (ADS)

Xiong, Yaokun; Zhou, Lifen; Zhao, Yonghong; Liu, Yun; Liu, Xia; Zhu, Genhua; Yan, Zhihong; Liu, Zhiyong

2018-01-01

Objective: To compare the effects of three extraction methods (ultrasound, reflux and percolation) on the contents of gentiopicroside, mangiferin, swertiamain, sweroside and oleanolic acid in Swertia mussotii Franch. Method: The contents of five components were determined by UPLC-ESI/MS. In the solvent system, eluent A was 0.05% (v: v) formic acid with 1mM/L ammonium acetate aqueous solution and eluent B was acetonitrile. Chromatographic separations were achieved using an Agilent EC-C18 column (4.6×100 mm, 2.7 um) at 30 °C. The flow rate was set at 0.8mL/min. The compound ionization was adopted at negative ionization mode by electro spray ionization (ESI). The quantification was performed in multiple reaction monitoring (MRM). Results: The linear ranges of swertiamarin, gentiopicroside, mangiferin, sweroside and oleanolic acid are 80∼7450 ng/mL, 103∼6600 ng/mL, 100∼8000 ng/mL, 130∼8450 ng/mL, 100∼7000 ng/mL, respectively. As a result, the content of oleanolic acid was the highest extracted by ultrasonic extraction and the content of mangiferin was the highest extracted by reflux extraction. For percolation extraction, the contents of five components were between ultrasound and reflux extraction. Conclusion: For five components, there are significant differences between the three different extraction methods. The results could provide a reference for the quality control of Swertia mussotii Franch and the research and development of new drugs.

Selective and cost-effective protocol to separate bioactive triterpene acids from plant matrices using alkalinized ethanol: Application to leaves of Myrtaceae species

PubMed Central

Lima, Adélia M. Belem; Siani, Antonio Carlos; Nakamura, Marcos Jun; D’Avila, Luiz Antonio

2015-01-01

Background: Triterpenes as betulinic (BA), oleanolic (OA) and ursolic acids (UA) have increasingly gained therapeutic relevance due to their wide scope of pharmacological activities. To fit large-scale demands, exploitable sources of these compounds have to be found and simple, cost-effective methods to extract them developed. Leaf material represents the best plant sustainable raw material. To obtain triterpene acid-rich extracts from leaves of Eugenia, Psidium and Syzygium species (Myrtaceae) by directly treating the dry plant material with alkalinized hydrated ethanol. This procedure was adapted from earlier methods to effect depolymerization of the leaf cutin. Materials and Methods: Extracts were prepared by shaking the milled dry leaves in freshly prepared 2% NaOH in 95% EtOH solution (1:4 w/v) at room temperature for 6 h. Working up the product in acidic aqueous medium led to clear precipitates in which BA, OA and UA were quantified by gas chromatography. Results: Pigment-free and low-polyphenol content extracts (1.2–2.8%) containing 6–50% of total triterpene acids were obtained for the six species assayed. UA (7–20%) predominated in most extracts, but BA preponderated in Eugenia florida (39%). Carried out in parallel, n-hexane defatted leaves led to up to 9% enhancement of total acids in the extracts. The hydroalcoholate treatment of Myrtaceae species dry leaves proved to be a cost-effective and environmentally friendly method to obtain triterpene acids, providing them be resistant to alkaline medium. These combined techniques might be applicable to other plant species and tissues. PMID:26246721

Evaluation of in-situ fatty acid extraction protocols for the analysis of staphylococcal cell membrane associated fatty acids by gas chromatography.

PubMed

Crompton, Marcus J; Dunstan, R Hugh

2018-05-01

The composition and integrity of the bacterial cytoplasmic membrane is critical to the survival of staphylococci in dynamic environments and it is important to investigate how the cell membrane responds to changes in the environmental conditions. The staphylococcal membrane differs from eukaryotic and many other bacterial cell membranes by having a high abundance of branch fatty acids and relatively few unsaturated fatty acids. The range of available methods for extraction and efficient analyses of staphylococcal fatty acids was initially appraised to identify the best potential procedures for appraisal. Staphylococcus aureus subsp. aureus Rosenbach (ATCC® 29213) was grown under optimal conditions to generate a cell biomass to compare the efficiencies of three approaches to extract and prepare methyl esters of the membrane fatty acids: (1) acidic direct transesterification of lipids, (2) modified basic direct transesterification of membrane lipids with adjusted reaction times and temperatures, and (3) base catalysed hydrolysis followed by acid catalysed esterification in two separate chemical reactions (MIDI process). All methods were able to extract fatty acids from the cell mass effectively where these lipids represented approximately 5% of the cellular dry mass. The acidic transesterification method had the least number of steps, the lowest coefficient of variation at 6.7% and good resistance to tolerating water. Basic transesterification was the least accurate method showing the highest coefficient of variation (26%). The MIDI method showed good recoveries, but had twice the number of steps and a coefficient of variation of 16%. It was also found that there was no need to use an anti-oxidant such as BHT for the protection of polyunsaturated fatty acids when the GC-MS injection liner was clean. It was concluded that the acidic transesterification procedures formed the most efficient and reproducible method for the analyses of staphylococcal membrane fatty acids. Crown Copyright © 2018. Published by Elsevier B.V. All rights reserved.

Detection of Chlorogenic Acid in Honeysuckle Using Infrared-Assisted Extraction Followed by Capillary Electrophoresis with UV Detector

PubMed Central

Tang, Zhuxing; Zang, Shuliang; Zhang, Xiangmin

2012-01-01

In this study, a novel infrared-assisted extraction method coupled capillary electrophoresis (CE) is employed to determine chlorogenic acid from a traditional Chinese medicine (TCM), honeysuckle. The effects of pH and the concentration of the running buffer, separation voltage, injection time, IR irradiation time, and anhydrous ethanol in the extraction concentration were investigated. The optimal conditions were as follows: extraction time, 30 min; extraction solvent, 80% (v/v) ethanol in water solution; and 50 mmol/L borate buffer (pH 8.7) was used as the running buffer at a separation voltage of 16 kV. The samples were injected electrokinetically at 16 kV for 8 s. Good linearity (r2 > 0.9996) was observed over the concentration ranges investigated, and the stability of the solutions was high. Recoveries of the chlorogenic acid were from 95.53% to 106.62%, and the relative standard deviation was below 4.1%. By using this novel IR-assisted extraction method, a higher extraction efficiency than those extracted with conventional heat-reflux extraction was found. The developed IR-assisted extraction method is simple, low-cost, and efficient, offering a great promise for the quick determination of active compounds in TCM. The results indicated that IR-assisted extraction followed by CE is a reliable method for quantitative analysis of active ingredient in TCM. PMID:22291060

Stability Test and Quantitative and Qualitative Analyses of the Amino Acids in Pharmacopuncture Extracted from Scolopendra subspinipes mutilans

PubMed Central

Cho, GyeYoon; Han, KyuChul; Yoon, JinYoung

2015-01-01

Objectives: Scolopendra subspinipes mutilans (S. subspinipes mutilans) is known as a traditional medicine and includes various amino acids, peptides and proteins. The amino acids in the pharmacopuncture extracted from S. subspinipes mutilans by using derivatization methods were analyzed quantitatively and qualitatively by using high performance liquid chromatography (HPLC) over a 12 month period to confirm its stability. Methods: Amino acids of pharmacopuncture extracted from S. subspinipes mutilans were derived by using O-phthaldialdehyde (OPA) & 9-fluorenyl methoxy carbonyl chloride (FMOC) reagent and were analyzed using HPLC. The amino acids were detected by using a diode array detector (DAD) and a fluorescence detector (FLD) to compare a mixed amino acid standard (STD) to the pharmacopuncture from centipedes. The stability tests on the pharmacopuncture from centipedes were done using HPLC for three conditions: a room temperature test chamber, an acceleration test chamber, and a cold test chamber. Results: The pharmacopuncture from centipedes was prepared by using the method of the Korean Pharmacopuncture Institute (KPI) and through quantitative analyses was shown to contain 9 amino acids of the 16 amino acids in the mixed amino acid STD. The amounts of the amino acids in the pharmacopuncture from centipedes were 34.37 ppm of aspartate, 123.72 ppm of arginine, 170.63 ppm of alanine, 59.55 ppm of leucine and 57 ppm of lysine. The relative standard deviation (RSD %) results for the pharmacopuncture from centipedes had a maximum value of 14.95% and minimum value of 1.795% on the room temperature test chamber, the acceleration test chamber and the cold test chamber stability tests. Conclusion: Stability tests on and quantitative and qualitative analyses of the amino acids in the pharmacopuncture extracted from centipedes by using derivatization methods were performed by using HPLC. Through research, we hope to determine the relationship between time and the concentrations of the amino acids in the pharmacopuncture extracted from centipedes. PMID:25830058

Development of new efficient method for isolation of phenolics from sea algae prior to their rapid resolution liquid chromatographic-tandem mass spectrometric determination.

PubMed

Klejdus, Bořivoj; Plaza, Merichel; Šnóblová, Marie; Lojková, Lea

2017-02-20

The extraction of phenolic compounds from 4 different sea algae samples, three brown algae (Cystoseira abies-marina, C. abies-marina grinded under cryogenic conditions with liquid nitrogen, Undaria pinnatifida and Sargassum muticum) and one red algae (Chondrus crispus) via solid phase extraction using micro-elution solid-phase extraction (μ-SPE) plate method was studied. Prior to μ-SPE, 50mg of algae with 80% methanol mixture was extracted in hyphenated series by various extraction techniques, such as pressurized liquid extraction and Ika Ultra-Turrax ® Tube Drive, in combination with ultrasound assisted extraction. The μ-SPE plate technique reduced the time of sample pre-treatment thanks to higher sensitivity and pre-concentration effect. Selected groups of benzoic acid derivatives (p-hydroxybenzoic, protocatechuic, gallic, vanillic, and syringic acids), hydroxybenzaldehydes (4-hydroxybenzaldehyde, and 3,4-dihydroxybenzaldehyde), and cinnamic acid derivatives (p-coumaric, caffeic, ferulic, sinapic, and chlorogenic acids) were determined using rapid resolution liquid chromatography coupled to mass spectrometry detection with negative ion electrospray ionization (RRLC-ESI-MS) using multiple reactions monitoring. LOQs of measured samples varied in the range 0.23-1.68ng/mL and LODs in the range 0.07-0.52ng/mL. The applied method allowed a simultaneous determination of phenolics (i.e. free, esters soluble in methanol, glycosides, and esters insoluble in methanol) in less than 5min (including alkaline or acidic hydrolysis of raw extracts) from sea algae extracts. Copyright © 2016 Elsevier B.V. All rights reserved.

A new standardized method for quantification of humic and fulvic acids in humic ores and commercial products.

PubMed

Lamar, Richard T; Olk, Daniel C; Mayhew, Lawrence; Bloom, Paul R

2014-01-01

Increased use of humic substances in agriculture has generated intense interest among producers, consumers, and regulators for an accurate and reliable method to quantify humic acid (HA) and fulvic acid (FA) in raw ores and products. Here we present a thoroughly validated method, the new standardized method for determination of HA and FA contents in raw humate ores and in solid and liquid products produced from them. The methods used for preparation of HA and FA were adapted according to the guidelines of the International Humic Substances Society involving alkaline extraction followed by acidification to separate HA from the fulvic fraction. This is followed by separation of FA from the fulvic fraction by adsorption on a nonionic macroporous acrylic ester resin at acid pH. It differs from previous methods in that it determines HA and FA concentrations gravimetrically on an ash-free basis. Critical steps in the method, e.g., initial test portion mass, test portion to extract volume ratio, extraction time, and acidification of alkaline extract, were optimized for maximum and consistent recovery of HA and FA. The method detection limits for HA and FA were 4.62 and 4.8 mg/L, respectively. The method quantitation limits for HA and FA were 14.7 and 15.3 mg/L, respectively.

Liquid chromatography-tandem mass spectrometry method for simultaneous quantification of azoxystrobin and its metabolites, azoxystrobin free acid and 2-hydroxybenzonitrile, in greenhouse-grown lettuce.

PubMed

Gautam, Maheswor; Fomsgaard, Inge S

2017-12-01

Lettuce is an important part of the diet in Europe. The permitted levels of pesticides in lettuce are strictly regulated and there is growing urge among food safety authorities to analyse pesticide metabolites as well. Azoxystrobin is one of pesticides that is frequently detected in lettuce. Although there are several analytical methods for the determination of azoxystrobin in lettuce, a sensitive method for the determination of its metabolites in lettuce is lacking. This study aimed at developing an extraction and LC-MS/MS method for the simultaneous determination of azoxystrobin, and its metabolites azoxystrobin free acid and 2-hydroxybenzonitrile in lettuce. Accelerated solvent extraction, QuEChERS extraction, and shaking extraction were compared using various solvents. The final method consisted of shaking freeze-dried sample in 0.1% formic acid in 80% aqueous acetonitrile. The selected method was validated by spiking each analyte at 125 ng/g and 500 ng/g. The method resulted in acceptable recovery for 2-hydroxybenzonitrile, azoxystrobin free acid, and azoxystrobin, with a RSD of <10%. The matrix-matched calibration curve for each analyte was linear over the range of quantification, with a correlation coefficient ≥0.98. The method was sensitive for the determination of 2-hydroxybenzonitrile, azoxystrobin free acid, and azoxystrobin, with limits of quantification of 0.36, 0.48, and 0.68 ng/g dry weight, respectively. The method was successfully applied to quantify 2-hydroxybenzonitrile, azoxystrobin free acid, and azoxystrobin in greenhouse-grown lettuce.

New method for the rapid extraction of natural products: efficient isolation of shikimic acid from star anise.

PubMed

Just, Jeremy; Deans, Bianca J; Olivier, Wesley J; Paull, Brett; Bissember, Alex C; Smith, Jason A

2015-05-15

A new, practical, rapid, and high-yielding process for the pressurized hot water extraction (PHWE) of multigram quantities of shikimic acid from star anise (Illicium verum) using an unmodified household espresso machine has been developed. This operationally simple and inexpensive method enables the efficient and straightforward isolation of shikimic acid and the facile preparation of a range of its synthetic derivatives.

Biological activities and chemical composition of lichens from Serbia

PubMed Central

Kosanic, Marijana; Rankovic, Branislav; Stanojkovic, Tatjana; Vasiljevic, Perica; Manojlovic, Nedeljko

2014-01-01

The aim of this study is to investigate chemical composition of acetone extracts of the lichens Parmelia arseneana and Acarospora fuscata and in vitro antioxidant, antimicrobial, and anticancer activities of these extracts and gyrophoric acid isolated from A. fuscata. The HPLC-UV method was used for the identification of secondary metabolites. Stictic acid, norstictic acid, gyrophoric acid, usnic acid, atranorin and chloroatranorin were identified in the A. fuscata. In P. arseneana, we detected stictic acid, norstictic acid, usnic acid and atranorin, while gyrophoric acid was not identified. Antioxidant activity was evaluated by measuring the scavenging capacity of tested samples on DPPH and superoxide anion radicals, reducing the power of samples and determination of total phenolic compounds in extracts. As a result of the study, gyrophoric acid was found to have the largest DPPH radical scavenging activity with an IC50 value of 105.75 µg/ml. Moreover, the tested samples had an effective superoxide anion radical scavenging and reducing power. The total content of phenol in extracts was determined as pyrocatechol equivalent. The antimicrobial activity was estimated by determination of the minimal inhibitory concentration by the broth microdilution method. The most active was also gyrophoric acid, with minimum inhibitory concentration values ranging from 0.019 to 1.25 mg/ml. Anticancer activity was tested against LS174 (human colon carcinoma cell line), A549 (human lung carcinoma cell line), Fem-x (malignant melanoma cell line), and a chronic myelogeneous leukaemia K562 cell line using the MTT method. Extract of P. arseneana expressed the strongest anticancer activity against all cell lines with IC50 values ranging from 11.61 to 47.06 µg/ml. PMID:26417336

Method of extracting coal from a coal refuse pile

DOEpatents

Yavorsky, Paul M.

1991-01-01

A method of extracting coal from a coal refuse pile comprises soaking the coal refuse pile with an aqueous alkali solution and distributing an oxygen-containing gas throughout the coal refuse pile for a time period sufficient to effect oxidation of coal contained in the coal refuse pile. The method further comprises leaching the coal refuse pile with an aqueous alkali solution to solubilize and extract the oxidized coal as alkali salts of humic acids and collecting the resulting solution containing the alkali salts of humic acids. Calcium hydroxide may be added to the solution of alkali salts of humic acid to form precipitated humates useable as a low-ash, low-sulfur solid fuel.

Fluid extraction

DOEpatents

Wai, Chien M.; Laintz, Kenneth E.

1999-01-01

A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a supercritical fluid solvent containing a chelating agent is described. The chelating agent forms chelates that are soluble in the supercritical fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is a fluorinated .beta.-diketone. In especially preferred embodiments the extraction solvent is supercritical carbon dioxide, and the chelating agent comprises a fluorinated .beta.-diketone and a trialkyl phosphate, or a fluorinated .beta.-diketone and a trialkylphosphine oxide. Although a trialkyl phosphate can extract lanthanides and actinides from acidic solutions, a binary mixture comprising a fluorinated .beta.-diketone and a trialkyl phosphate or a trialkylphosphine oxide tends to enhance the extraction efficiencies for actinides and lanthanides. The method provides an environmentally benign process for removing contaminants from industrial waste without using acids or biologically harmful solvents. The method is particularly useful for extracting actinides and lanthanides from acidic solutions. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

Application of ionic liquids based microwave-assisted simultaneous extraction of carnosic acid, rosmarinic acid and essential oil from Rosmarinus officinalis.

PubMed

Liu, Tingting; Sui, Xiaoyu; Zhang, Rongrui; Yang, Lei; Zu, Yuangang; Zhang, Lin; Zhang, Ying; Zhang, Zhonghua

2011-11-25

An ionic liquid based microwave-assisted simultaneous extraction and distillation (ILMSED) method has been developed for the effective extraction of carnosic acid (CA), rosmarinic acid (RA) and essential oil (EO) from Rosmarinus officinalis. A series of 1-alkyl-3-methylimidazolium ionic liquids differing in composition of anion and cation were evaluated for extraction yield in this work. The results obtained indicated that the anions and cations of ionic liquids had influences on the extraction of CA and RA, 1.0M 1-octyl-3-methylimidazolium bromide ([C8mim]Br) solution was selected as solvent. In addition, the ILMSED procedures for the three target ingredients were optimized and compared with other conventional extraction techniques. ILMSED gave the best result due to the highest extraction yield within the shortest extraction time for CA and RA. The novel process developed offered advantages in term of yield and selectivity of EO and shorter isolation time (20 min in comparison of 4h of hydrodistillation), and provides a more valuable EO (with high amount of oxygenated compounds). The microstructures and chemical structures of rosemary samples before and after extraction were also investigated. Moreover, the proposed method was validated by the stability, repeatability and recovery experiments. The results indicated that the developed ILMSED method provided a good alternative for the both extraction of non-volatile compounds (CA and RA) and EO from rosemary as well as other herbs. Copyright © 2011 Elsevier B.V. All rights reserved.

[The isolation of organic compounds from hydrosulfuric mineral waters with the use of the extractive freezing-out technique with centrifugation].

PubMed

Bekhterev, V N; Kabina, E A

The mineral waters, enriched with organic substances find extensive application in balneotherapy. The fast and efficient methods for the identification and quantitative measurement of organic compounds (in the first place, organic acids) in such waters need to be developed for the estimation of their quality and biological activity. The objective of the present study was to elaborate a gas chromatographic method for the determination of monobasic carbonic acids in sulfide-containing mineral waters by means of extractive freezing-out in combination with the application of the centrifugal forces for the elucidation of the metrological characteristics of the compounds of interest. The secondary objective was to estimate the prospects for the application of the method of interest for determining the dissolved organic compounds in mineral waters. The following carbonic acids were used for the purposes of the study: acetic acid (analytical grade), Russia; propionic grade (extra pure), Ferak, Germany; butyric acid (pure), Russia; valeric acid (pure), Russia; caproic acid (pure), Russia; oenanthic acid (pure), Russia; and caprylic acid (pure), Russia). Acetonitrile («O» grade), Russia, was used as the extracting agent. The LV-210 analytical balance (Russia) was used to prepare the model and standard solutions of the organic compounds and to determine their mass. The extracts and standard mixture were investigated by the gas chromatographic technique with the use of the Kristallyuks apparatus («Meta-Khrom», Russia) equipped with the flame ionization detector and the capillary column. Extractive freezing-out in the combination with centrifugation was performed with the laboratory installation for this purpose. Under the model conditions, a single extractive freezing-out procedure with the centrifugation of the sample made it possible to reach the 22-37-fold concentration of C2-C8 monobasic carbonic acids during their transfer from water into acetonitrile. The metrological parameters of the proposed procedure for gas-chromatographic determination of the aforementioned acids in hydrosulfuric mineral waters were estimated. The limit of detection of acetic and propionic acids has been 0,2 mg/l, that for butyric acid 0,1 mg/l, for valeric, caproic, oenanthic and caprylic acids 0,05 mg/l. We failed to identify C2-C8 carbonic acids in hydrosulfuric water from the 6T well of the field Matsesta fields. The investigation of the extracts obtained by the proposed extraction procedure with the use of the newly developed variant of high performance liquid chromatography (HPLC) with diode-matrix detection revealed the presence of various amounts of unknown organic substances. The UV-spectrum of one of those components was obtained which made it possible to conjecture its molecular structure. The procedure for the sample preparation and the following determination of organic acids in water is simple, carried out in a single stage, and does not impose special requirements to the qualification of the researcher. It allows to describe the newly developed technique as a rapid test method. Along with it, realization of extraction in the negative temperature mode reduces the risk of decomposition of the thermally unstable chemical compounds being extracted and reduces volatility of the organic solvents being used. The technology of the method does not demand a special laboratory glassware and expendables.

Development and validation of an RP-HPLC method for quantitative determination of vanillin and related phenolic compounds in Vanilla planifolia.

PubMed

Sinha, Arun Kumar; Verma, Subash Chandra; Sharma, Upendra Kumar

2007-01-01

A simple and fast method was developed using RP-HPLC for separation and quantitative determination of vanillin and related phenolic compounds in ethanolic extract of pods of Vanilla planifolia. Ten phenolic compounds, namely 4-hydroxybenzyl alcohol, vanillyl alcohol, 3,4-dihydroxybenzaldehyde, 4-hydroxybenzoic acid, vanillic acid, 4-hydroxybenzaldehyde, vanillin, p-coumaric acid, ferulic acid, and piperonal were quantitatively determined using ACN, methanol, and 0.2% acetic acid in water as a mobile phase with a gradient elution mode. The method showed good linearity, high precision, and good recovery of compounds of interest. The present method would be useful for analytical research and for routine analysis of vanilla extracts for their quality control.

Antimicrobial activity and chemical analysis of Microlicia hatschbachii Wurdack (Melastomataceae) extract.

PubMed

Cassiano, Dayse S A; Pacheco, Alessandra G M; da Costa, Mateus M; Almeida, Jackson R G S; Vieira, Ivo J C; Branco, Alexsandro

2014-01-01

Aerial parts of Microlicia hatschbachii were extracted with hexane, and the extract was evaluated for antimicrobial activity by a broth dilution method. After phytochemical procedures: GC-MS identified aliphatic alkanes, carboxylic acids and methyl esters of long-chain fatty acids; and two diterpenoids [labd-8(17)-en-15-oic acid and labd-8(17),13-dien-15-oic acid] were identified by (1)H and (13)C NMR. The antimicrobial activity of the hexane extract could be attributed to the presence of labdanes. This identification is the first reported occurrence of labdane diterpenes in the Melastomataceae family.

Mathematical modelling for extraction of oil from Dracocephalum kotschyi seeds in supercritical carbon dioxide.

PubMed

Sodeifian, Gholamhossein; Sajadian, Seyed Ali; Honarvar, Bizhan

2018-04-01

Extraction of oil from Dracocephalum kotschyi Boiss seeds using supercritical carbon dioxide was designed using central composite design to evaluate the effect of various operating parameters including pressure, temperature, particle size and extraction time on the oil yield. Maximum extraction yield predicted from response surface method was 71.53% under the process conditions with pressure of 220 bar, temperature of 35 °C, particle diameter of 0.61 mm and extraction time of 130 min. Furthermore, broken and intact cells model was utilised to consider mass transfer kinetics of extracted natural materials. The results revealed that the model had a good agreement with the experimental data. The oil samples obtained via supercritical and solvent extraction methods were analysed by gas chromatography. The most abundant acid was linolenic acid. The results analysis showed that there was no significant difference between the fatty acid contents of the oils obtained by the supercritical and solvent extraction techniques.

Determination of Acid and Neutral Cannabinoids in Extracts of Different Strains of Cannabis sativa Using GC-FID.

PubMed

Ibrahim, Elsayed A; Gul, Waseem; Gul, Shahbaz W; Stamper, Brandon J; Hadad, Ghada M; Abdel Salam, Randa A; Ibrahim, Amany K; Ahmed, Safwat A; Chandra, Suman; Lata, Hemant; Radwan, Mohamed M; ElSohly, Mahmoud A

2018-03-01

Cannabis ( Cannabis sativa L.) is an annual herbaceous plant that belongs to the family Cannabaceae. Trans -Δ 9 -tetrahydrocannabinol (Δ 9 -THC) and cannabidiol (CBD) are the two major phytocannabinoids accounting for over 40% of the cannabis plant extracts, depending on the variety. At the University of Mississippi, different strains of C. sativa, with different concentration ratios of CBD and Δ 9 -THC, have been tissue cultured via micropropagation and cultivated. A GC-FID method has been developed and validated for the qualitative and quantitative analysis of acid and neutral cannabinoids in C. sativa extracts. The method involves trimethyl silyl derivatization of the extracts. These cannabinoids include tetrahydrocannabivarian, CBD, cannabichromene, trans -Δ 8 -tetrahydrocannabinol, Δ 9 -THC, cannabigerol, cannabinol, cannabidiolic acid, cannabigerolic acid, and Δ 9 -tetrahydrocannabinolic acid-A. The concentration-response relationship of the method indicated a linear relationship between the concentration and peak area ratio with R 2  > 0.999 for all 10 cannabinoids. The precision and accuracy of the method were found to be ≤ 15% and ± 5%, respectively. The limit of detection range was 0.11 - 0.19 µg/mL, and the limit of quantitation was 0.34 - 0.56 µg/mL for all 10 cannabinoids. The developed method is simple, sensitive, reproducible, and suitable for the detection and quantitation of acidic and neutral cannabinoids in different extracts of cannabis varieties. The method was applied to the analysis of these cannabinoids in different parts of the micropropagated cannabis plants (buds, leaves, roots, and stems). Georg Thieme Verlag KG Stuttgart · New York.

[Technological process of cell disruption for extracting astaxanthin from Phaffia rhodozyma by acid method under autoclave conditions].

PubMed

Lu, Baoju; Xiao, Anfeng; Lil, Lijun; Ni, Hui; Cai, Huinong; Su, Wenjin

2008-07-01

Phaffia rhodozyma is one of the organisms for production of astaxanthin, and the key process for extracting intracellular astaxanthin is cell disruption. In this work, cell disruption for extracting astaxanthin from Phaffia rhodozyma was studied with autoclave method at low acid concentration. The optimum disrupting conditions were: autoclave pressure 0.1 MPa, 121 degrees C; hydrochloric acid concentration 0.5 mol/L; liquid to material ratio (V/W) 30 mL/g dry cell weight and disruption time 2 min. Under the optimum conditions, medium scale experiment showed that astaxanthin and total carotenoids recovery from Phaffia rhodozyma were (84.8 +/- 3.2)% and (93.3 +/- 2)%, respectively. This new method can lead to no poisonous residues and get high extraction yield, which have good prospects to be put into industrial production.

A rapid miniaturized residue analytical method for the determination of zoxamide and its two acid metabolites in ginseng roots using UPLC-MS/MS.

PubMed

Podhorniak, Lynda V

2014-04-30

A miniaturized residue method was developed for the analysis of the fungicide zoxamide and its metabolites in dried ginseng root. The zoxamide metabolites, 3,5-dichloro-1,4-benzenedicarboxylic acid (DCBC) and 3,5-dichloro-4-hydroxymethylbenzoic acid (DCHB), are small acid molecules that have not been previously extracted from the ginseng matrix with common multiresidue methods. The presented extraction method effectively and rapidly recovers both the zoxamide parent compound and its acid metabolites from fortified ginseng root. The metabolites are extracted with an alkaline glycine buffer and the aqueous ginseng mixture is partitioned with ethyl acetate. In addition, this method avoids the use of derivatization of the small acid molecules by using UPLC-MS/MS instrumental analysis. In a quantitative validation of the analytical method at three levels for zoxamide (0.007 (LOD), 0.02 (LOQ), and 0.2 mg/kg) and four levels (0.07 (LOD), 0.2 (LOQ), and 0.6 and 6 mg/kg) for both metabolites, acceptable method performances were achieved with recoveries ranging from 86 to 107% (at levels of LOQ and 3×, 10×, and 30× the LOQ) with <20% RSD for the three analytes in accordance with international guidelines.1.

Analgesic, antibacterial and central nervous system depressant activities of Albizia procera leaves.

PubMed

Khatoon, Mst Mahfuza; Khatun, Mst Hajera; Islam, Md Ekramul; Parvin, Mst Shahnaj

2014-04-01

To ascertain analgesic, antibacterial and central nervous system (CNS) depressant activities of ethyl acetate, dichloromethane and carbon tetrachloride fractions of methanol extract of Albizia procera (A. procera) leaves. Leaves extracts of A. procera were tested for analgesic activity by acetic acid induced and formalin test method in mice. The in vitro antibacterial activity was performed by agar well diffusion method. CNS depressant activity was evaluated by hole cross and open field tests. All the extracts at 200 mg/kg exhibited significant (P<0.01) analgesic activity in acetic acid induced and formalin tests method in mice. Analgesic activity of the ethyl acetate fraction was almost same like as standard drug indomethacin in acetic acid induced method. The CNS depressant activity of the extracts at 500 mg/kg was comparable to the positive control diazepam as determined by hole cross and open field test method. The extracts exhibited moderate antimicrobial activity against all the tested microorganisms (Staphylococcus aureus, Bacillus cereus, Pseudomonas aeruginosa, Esherichia coli, Shigella soneii, Shigella boydii) at concentration of 0.8 mg/disc. The measured diameter of zone of inhibition for the extracts was within the range of 7 to 12 mm which was less than the standard kanamycin (16-24 mm). It is concluded that all the extracts possess potential analgesic and CNS depressants activity. This study also showed that different fractions of methanol extract could be potential sources of new antimicrobial agents.

Ulcer healing activity of Mumijo aqueous extract against acetic acid induced gastric ulcer in rats

PubMed Central

Shahrokhi, Nader; Keshavarzi, Zakieh; Khaksari, Mohammad

2015-01-01

Objective: Gastric ulcer is an important clinical problem, chiefly due to extensive use of some drugs. The aim was to assess the activity of Mumijo extract (which is used in traditional medicine) against acetic acid induced gastric ulcer in rats. Materials and Methods: The aqueous extract of Mumijo was prepared. Animals were randomly (n = 10) divided into four groups: Control, sham-operated group (received 0.2 ml of acetic acid to induce gastric ulcer), Mumijo (100 mg/kg/daily) were given for 4 days postacetic acid administration, and ranitidine group (20 mg/kg). The assessed parameters were pH and pepsin levels (by Anson method) of gastric contents and gastric histopathology. Ranitidine was used as reference anti-ulcer drug. Results: The extract (100 mg/kg/daily, p.o.) inhibited acid acetic-induced gastric ulceration by elevating its pH versus sham group (P < 0.01) and decreasing the pepsin levels compared to standard drug, ranitidine (P < 0.05). The histopathology data showed that the treatment with Mumijo extract had a significant protection against all mucosal damages. Conclusion: Mumijo extract has potent antiulcer activity. Its anti-ulcer property probably acts via a reduction in gastric acid secretion and pepsin levels. The obtained results support the use of this herbal material in folk medicine. PMID:25709338

Ascorbic acid and tannins from Emblica officinalis Gaertn. Fruits--a revisit.

PubMed

Majeed, Muhammed; Bhat, Beena; Jadhav, Atul N; Srivastava, Jyotish S; Nagabhushanam, Kalyanam

2009-01-14

The fruits of Emblica officinalis Gaertn. (Euphorbiaceae), also known as amla in Ayurveda, are considered to be a rich source of ascorbic acid. However, the antioxidant activities exhibited by E. officinalis extract are superior to those of ascorbic acid itself. Low molecular hydrolyzable tannins emblicanins A and B have been suggested in the earlier literature to be the contributory antioxidant molecules in the extract. This work finds no evidence for the presence of emblicanins A and B in the extract. In addition, the high content of ascorbic acid is also questionable due to previous nonidentification of coeluting mucic acid gallates. This paper reports a new HPLC method to detect even trace amounts of ascorbic acid in E. officinalis fruit juice or extract.

Predicting nucleic acid binding interfaces from structural models of proteins

PubMed Central

Dror, Iris; Shazman, Shula; Mukherjee, Srayanta; Zhang, Yang; Glaser, Fabian; Mandel-Gutfreund, Yael

2011-01-01

The function of DNA- and RNA-binding proteins can be inferred from the characterization and accurate prediction of their binding interfaces. However the main pitfall of various structure-based methods for predicting nucleic acid binding function is that they are all limited to a relatively small number of proteins for which high-resolution three dimensional structures are available. In this study, we developed a pipeline for extracting functional electrostatic patches from surfaces of protein structural models, obtained using the I-TASSER protein structure predictor. The largest positive patches are extracted from the protein surface using the patchfinder algorithm. We show that functional electrostatic patches extracted from an ensemble of structural models highly overlap the patches extracted from high-resolution structures. Furthermore, by testing our pipeline on a set of 55 known nucleic acid binding proteins for which I-TASSER produces high-quality models, we show that the method accurately identifies the nucleic acids binding interface on structural models of proteins. Employing a combined patch approach we show that patches extracted from an ensemble of models better predicts the real nucleic acid binding interfaces compared to patches extracted from independent models. Overall, these results suggest that combining information from a collection of low-resolution structural models could be a valuable approach for functional annotation. We suggest that our method will be further applicable for predicting other functional surfaces of proteins with unknown structure. PMID:22086767

Solid-phase extraction of acidic herbicides.

PubMed

Wells, M J; Yu, L Z

2000-07-14

A discussion of solid-phase extraction method development for acidic herbicides is presented that reviews sample matrix modification, extraction sorbent selection, derivatization procedures for gas chromatographic analysis, and clean-up procedures for high-performance liquid chromatographic analysis. Acidic herbicides are families of compounds that include derivatives of phenol (dinoseb, dinoterb and pentachlorophenol), benzoic acid (acifluorfen, chloramben, dicamba, 3,5-dichlorobenzoic acid and dacthal--a dibenzoic acid derivative), acetic acid [2,4-dichlorophenoxyacetic acid (2,4-D), 4-chloro-2-methylphenoxyacetic acid (MCPA) and 2,4,5-trichlorophenoxyacetic acid (2,4,5-T)], propanoic acid [dichlorprop, fluazifop, haloxyfop, 2-(4-chloro-2-methylphenoxy)propanoic acid (MCPP) and silvex], butanoic acid [4-(2,4-dichlorophenoxy)butanoic acid (2,4-DB) and 4-(4-chloro-2-methylphenoxy)butanoic acid (MCPB)], and other miscellaneous acids such as pyridinecarboxylic acid (picloram) and thiadiazine dioxide (bentazon).

Sequential extractions of selenium soils from Stewart Lake: total selenium and speciation measurements with ICP-MS detection.

PubMed

Ponce de León, Claudia A; DeNicola, Katie; Montes Bayón, Maria; Caruso, Joseph A

2003-06-01

Different techniques have been employed in order to evaluate the most efficient procedure for the extraction of selenium from soil as required for speciation. Selenium contaminated sediments from Stewart Lake Wetland, California were used. A strong acid mineralization of the samples gives quantitative total selenium, which is then used to estimate recoveries for the milder extraction methods. The different extraction methodologies involve the sequential use of water, buffer (phosphate, pH 7) and either acid solution (e.g. HNO3 or HCl) or basic solutions (e.g. ammonium acetate, NaOH or TMAH). Pyrophosphate extraction was also evaluated and showed that selenium was not associated with humic acids. The extractants were subsequently analyzed by size exclusion chromatography (SEC) with UV (254 and 400 nm) and on-line ICP-MS detection; anion exchange chromatography, and ion-pair reversed phase chromatography with ICP-MS detection. For sequential extractions the extraction efficiencies showed that the basic extractions were more efficient than the acidic. The difference between the acidic and the basic extraction efficiency is carried to the sulfite extraction, suggesting that whatever is not extracted by the acid is subsequently extracted by the sulfite. The species identified with the different chromatographies were selenate, selenite, elemental selenium and some organic selenium.

Two-step extraction method for lead isotope fractionation to reveal anthropogenic lead pollution.

PubMed

Katahira, Kenshi; Moriwaki, Hiroshi; Kamura, Kazuo; Yamazaki, Hideo

2018-05-28

This study developed the 2-step extraction method which eluted the Pb adsorbing on the surface of sediments in the first solution by aqua regia and extracted the Pb absorbed inside particles into the second solution by mixed acid of nitric acid, hydrofluoric acid and hydrogen peroxide solution. We applied the method to sediments in the enclosed water area and found out that the isotope ratios of Pb in the second solution represented those of natural origin. This advantage of the method makes it possible to distinguish the Pb between natural origin and anthropogenic source on the basis of the isotope ratios. The results showed that the method was useful to discuss the Pb sources and that anthropogenic Pb in the sediment samples analysed was mainly derived from China because of transboundary air pollution.

[Inhibition of Linseed Oil Autooxidation by Essential Oils and Extracts from Spice Plants].

PubMed

Misharina, T A; Alinkina, E S; Terenina, M B; Krikunova, N I; Kiseleva, V I; Medvedeva, I B; Semenova, M G

2015-01-01

Clove bud essential oil, extracts from ginger, pimento and black pepper, or ascorbyl palmytate were studied as natural antioxidants for the inhibition of autooxidation of polyunsaturated fatty acids in linseed oil. Different methods were used to estimate antioxidant efficiency. These methods are based on the following parameters: peroxide values; peroxide concentration; content of degradation products of unsaturated fatty acid peroxides, which acted with thiobarbituric acid; diene conjugate content; the content of volatile compounds that formed as products of unsaturated fatty acid peroxide degradation; and the composition of methyl esters of fatty acids in samples of oxidized linseed oil.

Method for purifying bidentate organophosphorus compounds

DOEpatents

Schulz, Wallace W.

1977-01-01

Bidentate organophosphorus compounds useful for extracting actinide elements from acidic nuclear waste solutions are purified of undesirable acidic impurities by contacting the compounds with ethylene glycol which preferentially extracts the impurities found in technical grade bidentate compounds.

Sensitive assay, based on hydroxy fatty acids from lipopolysaccharide lipid A, for Gram-negative bacteria in sediments.

PubMed Central

Parker, J H; Smith, G A; Fredrickson, H L; Vestal, J R; White, D C

1982-01-01

Biochemical measures have provided insight into the biomass and community structure of sedimentary microbiota without the requirement of selection by growth or quantitative removal from the sediment grains. This study used the assay of the hydroxy fatty acids released from the lipid A of the lipopolysaccharide in sediments to provide an estimate of the gram-negative bacteria. The method was sensitive to picomolar amounts of hydroxy fatty acids. The recovery of lipopolysaccharide hydroxy fatty acids from organisms added to sediments was quantitative. The lipids were extracted from the sediments with single-phase chloroform-methanol extraction. The lipid-extraction residue was hydrolyzed in 1 N HCl, and the hydroxy fatty acids of the lipopolysaccharide were recovered in chloroform for analysis by gas-liquid chromatography. This method proved to be about fivefold more sensitive than the classical phenol-water or trichloroacetic acid methods when applied to marine sediments. By examination of the patterns of hydroxy fatty acids, it was also possible to help define the community structure of the sedimentary gram-negative bacteria. PMID:6817712

Electromembrane extraction using two separate cells: A new design for simultaneous extraction of acidic and basic compounds.

PubMed

Nojavan, Saeed; Asadi, Sakine

2016-02-01

Simultaneous extraction of acidic and basic analytes from a sample is seen to be a challenging task. In this work, a novel and efficient electromembrane extraction (EME) method based on two separate cells was applied to simultaneously extract and preconcentrate two acidic drugs (naproxen and ibuprofen) along with a basic drug (ketamine). Once both cells were filled with the sample solution, basic drug was extracted from one cell with the other cell used to extract acidic drugs. The employed supported liquid membranes for the extraction of acidic and basic drugs were 2-ethyl hexanol and 1-octanol, respectively. Under an applied potential of 250 V in the course of the extraction process, acidic, and basic drugs were extracted from a 3.0 mL aqueous sample solution into 25 μL acceptor solutions. The pH values of the donor and acceptor solutions in the cathodic cell were 5.0 and 1.5, respectively, the corresponding values in the anodic cell were, however, 8.0 and 12.5, respectively. The rates of recovery obtained within 20 min of extraction time at a stirring rate of 750 rpm ranged from 45 to 54%. With correlation coefficients ranging from 0.990 to 0.996, the proposed EME technique provided good linearity over a concentration range of 20-1000 ng/mL. The LOD for all drugs was found to be 6.7 ng/mL, while reproducibility ranged from 7 to 12% (n = 5). Finally, applying the proposed method to determine and quantify the drugs in urine and wastewater samples, satisfactory results were achieved. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of gold, indium, tellurium and thallium in the same sample digest of geological materials by atomic-absorption spectroscopy and two-step solvent extraction

USGS Publications Warehouse

Hubert, A.E.; Chao, T.T.

1985-01-01

A rock, soil, or stream-sediment sample is decomposed with hydrofluoric acid, aqua regia, and hydrobromic acid-bromine solution. Gold, thallium, indium and tellurium are separated and concentrated from the sample digest by a two-step MIBK extraction at two concentrations of hydrobromic add. Gold and thallium are first extracted from 0.1M hydrobromic acid medium, then indium and tellurium are extracted from 3M hydrobromic acid in the presence of ascorbic acid to eliminate iron interference. The elements are then determined by flame atomic-absorption spectrophotometry. The two-step solvent extraction can also be used in conjunction with electrothermal atomic-absorption methods to lower the detection limits for all four metals in geological materials. ?? 1985.

Analgesic, antibacterial and central nervous system depressant activities of Albizia procera leaves

PubMed Central

Khatoon, Mst. Mahfuza; Khatun, Mst. Hajera; Islam, Md. Ekramul; Parvin, Mst. Shahnaj

2014-01-01

Objective To ascertain analgesic, antibacterial and central nervous system (CNS) depressant activities of ethyl acetate, dichloromethane and carbon tetrachloride fractions of methanol extract of Albizia procera (A. procera) leaves. Methods Leaves extracts of A. procera were tested for analgesic activity by acetic acid induced and formalin test method in mice. The in vitro antibacterial activity was performed by agar well diffusion method. CNS depressant activity was evaluated by hole cross and open field tests. Results All the extracts at 200 mg/kg exhibited significant (P<0.01) analgesic activity in acetic acid induced and formalin tests method in mice. Analgesic activity of the ethyl acetate fraction was almost same like as standard drug indomethacin in acetic acid induced method. The CNS depressant activity of the extracts at 500 mg/kg was comparable to the positive control diazepam as determined by hole cross and open field test method. The extracts exhibited moderate antimicrobial activity against all the tested microorganisms (Staphylococcus aureus, Bacillus cereus, Pseudomonas aeruginosa, Esherichia coli, Shigella soneii, Shigella boydii) at concentration of 0.8 mg/disc. The measured diameter of zone of inhibition for the extracts was within the range of 7 to 12 mm which was less than the standard kanamycin (16-24 mm). Conclusions It is concluded that all the extracts possess potential analgesic and CNS depressants activity. This study also showed that different fractions of methanol extract could be potential sources of new antimicrobial agents. PMID:25182551

Actinide extraction methods

DOEpatents

Peterman, Dean R [Idaho Falls, ID; Klaehn, John R [Idaho Falls, ID; Harrup, Mason K [Idaho Falls, ID; Tillotson, Richard D [Moore, ID; Law, Jack D [Pocatello, ID

2010-09-21

Methods of separating actinides from lanthanides are disclosed. A regio-specific/stereo-specific dithiophosphinic acid having organic moieties is provided in an organic solvent that is then contacted with an acidic medium containing an actinide and a lanthanide. The method can extend to separating actinides from one another. Actinides are extracted as a complex with the dithiophosphinic acid. Separation compositions include an aqueous phase, an organic phase, dithiophosphinic acid, and at least one actinide. The compositions may include additional actinides and/or lanthanides. A method of producing a dithiophosphinic acid comprising at least two organic moieties selected from aromatics and alkyls, each moiety having at least one functional group is also disclosed. A source of sulfur is reacted with a halophosphine. An ammonium salt of the dithiophosphinic acid product is precipitated out of the reaction mixture. The precipitated salt is dissolved in ether. The ether is removed to yield the dithiophosphinic acid.

Identification of fermentation inhibitors in wood hydrolyzates and removal of inhibitors by ion exchange and liquid-liquid extraction

NASA Astrophysics Data System (ADS)

Luo, Caidian

1998-12-01

Common methods employed in the ethanol production from biomass consist of chemical or enzymatic degradation of biomass into sugars and then fermentation of sugars into ethanol or other chemicals. However, some degradation products severely inhibit the fermentation processes and substantially reduce the efficiency of ethanol production. How to remove inhibitors from the reaction product mixture and increase the production efficiency are critical in the commercialization of any processes of energy from biomass. The present study has investigated anion exchange and liquid-liquid extraction as potential methods for inhibitor removal. An analytical method has been developed to identify the fermentation inhibitors in a hydrolyzate. The majority of inhibitors present in hybrid poplar hydrolyzate have positively been identified. Ion exchange with weak basic Dowex-MWA-1 resin has been proved to be an effective mean to remove fermentation inhibitors from hybrid poplar hydrolyzate and significantly increase the fermentation productivity. Extraction with n-butanol might be a preferred way to remove inhibitors from wood hydrolyzates and improve the fermentability of sugars in the hydrolyzates. n-Butanol also removes some glucose, mannose and xylose from the hydrolyzate. Inhibitor identification reveals that lignin and sugar degradation compounds including both aromatic and aliphatic aldehydes and carboxylic acids formed in hydrolysis, plus fatty acids and other components from wood extractives are major fermentation inhibitors in Sacchromyces cerevisiae fermentation. There are 35 components identified as fermentation inhibitors. Among them, 4-hydroxy benzoic acid, 3,4-dihydroxy benzoic acid, syringic acid, syringaldehyde, and ferulic acid are among the most abundant aromatic inhibitors in hybrid poplar hydrolyzate. The conversion of aldehyde groups into carboxylic acid groups in the nitric acid catalyzed hydrolysis reduces the toxicity of the hydrolyzate. A wide spectrum of aliphatic acids has been identified in the wood hydrolyzate studied. They are potential fermentation inhibitors probably similar to acetic acid. Ethyl acetate extraction has also been demonstrated to be a possible method to remove fermentation inhibitors from hydrolyzates. (Abstract shortened by UMI.)

Method for liquid chromatographic extraction of strontium from acid solutions

DOEpatents

Horwitz, E. Philip; Dietz, Mark L.

1992-01-01

A method and apparatus for extracting strontium and technetium values from biological, industrial and environmental sample solutions using a chromatographic column is described. An extractant medium for the column is prepared by generating a solution of a diluent containing a Crown ether and dispersing the solution on a resin substrate material. The sample solution is highly acidic and is introduced directed to the chromatographic column and strontium or technetium is eluted using deionized water.

Comparison of the free and bound phenolic profiles and cellular antioxidant activities of litchi pulp extracts from different solvents

PubMed Central

2014-01-01

Background The phenolic contents and antioxidant activities of fruits could be underestimated if the bound phenolic compounds are not considered. In the present study, the extraction efficiencies of various solvents were investigated in terms of the total content of the free and bound phenolic compounds, as well as the phenolic profiles and antioxidant activities of the extracts. Methods Five different solvent mixtures were used to extract the free phenolic compounds from litchi pulp. Alkaline and acidic hydrolysis methods were compared for the hydrolysis of bound phenolic compounds from litchi pulp residue. The phenolic compositions of the free and bound fractions from the litchi pulp were identified using HPLC-DAD. The antioxidant activities of the litchi pulp extracts were determined by oxygen radical absorbance capacity (ORAC) and cellular antioxidant activity (CAA) assays. Results Of the solvents tested, aqueous acetone extracted the largest amount of total free phenolic compounds (210.7 mg GAE/100 g FW) from litchi pulp, followed sequentially by aqueous mixtures of methanol, ethanol and ethyl acetate, and water itself. The acid hydrolysis method released twice as many bound phenolic compounds as the alkaline hydrolysis method. Nine phenolic compounds were detected in the aqueous acetone extract. In contrast, not all of these compounds were found in the other four extracts. The classification and content of the bound phenolic compounds released by the acid hydrolysis method were higher than those achieved by the alkaline hydrolysis. The aqueous acetone extract showing the highest ORAC value (3406.9 μmol TE/100 g FW) for the free phenolic extracts. For the CAA method, however, the aqueous acetone and methanol extracts (56.7 and 55.1 μmol QE/100 g FW) showed the highest levels of activity of the five extracts tested. The ORAC and CAA values of the bound phenolic compounds obtained by acid hydrolysis were 2.6- and 1.9-fold higher than those obtained using the alkaline hydrolysis method. Conclusions The free and bound phenolic contents and profiles and antioxidant activities of the extracts were found to be dependent on the extraction solvent used. Litchi exhibited good cellular antioxidant activity and could be a potentially useful natural source of antioxidants. PMID:24405977

Antioxidant and antimicrobial activities of ethyl acetate extract, fractions and compounds from stem bark of Albizia adianthifolia (Mimosoideae).

PubMed

Tamokou, Jean de Dieu; Simo Mpetga, Deke James; Keilah Lunga, Paul; Tene, Mathieu; Tane, Pierre; Kuiate, Jules Roger

2012-07-18

Albizia adianthifolia is used traditionally in Cameroon to treat several ailments, including infectious and associated diseases. This work was therefore designed to investigate the antioxidant and antimicrobial activities of ethyl acetate extract, fractions and compounds isolated from the stem bark of this plant. The plant extract was prepared by maceration in ethyl acetate. Its fractionation was done by column chromatography and the structures of isolated compounds were elucidated using spectroscopic data in conjunction with literature data. The 1,1-diphenyl-2-picrylhydrazyl (DPPH) and trolox equivalent antioxidant capacity (TEAC) assays were used to detect the antioxidant activity. Broth micro-dilution method was used for antimicrobial test. Total phenol content was determined spectrophotometrically in the extracts by using Folin-Ciocalteu method. The fractionation of the extract afforded two known compounds: lupeol (1) and aurantiamide acetate (2) together with two mixtures of fatty acids: oleic acid and n-hexadecanoic acid (B₁); n-hexadecanoic acid, octadecanoic acid and docosanoic acid (B₂). Aurantiamide acetate was the most active compound. The total phenol concentration expressed as gallic acid equivalents (GAE) was found to vary from 1.50 to 13.49 μg/ml in the extracts. The antioxidant activities were well correlated with the total phenol content (R² = 0.946 for the TEAC method and R² = 0.980 for the DPPH free-radical scavenging assay). Our results clearly reveal that the ethyl acetate extract from the stem bark of A. adianthifolia possesses antioxidant and antimicrobial principles. The antioxidant activity of this extract as well as that of compound 2 are being reported herein for the first time. These results provide promising baseline information for the potential use of this plant as well as compound 2 in the treatment of oxidative damage and infections associated with the studied microorganisms.

High-resolution gas chromatography/mass spectrometry method for characterization and quantitative analysis of ginkgolic acids in Ginkgo biloba plants, extracts, and dietary supplements.

PubMed

Wang, Mei; Zhao, Jianping; Avula, Bharathi; Wang, Yan-Hong; Avonto, Cristina; Chittiboyina, Amar G; Wylie, Philip L; Parcher, Jon F; Khan, Ikhlas A

2014-12-17

A high-resolution gas chromatography/mass spectrometry (GC/MS) with selected ion monitor method focusing on the characterization and quantitative analysis of ginkgolic acids (GAs) in Ginkgo biloba L. plant materials, extracts, and commercial products was developed and validated. The method involved sample extraction with (1:1) methanol and 10% formic acid, liquid-liquid extraction with n-hexane, and derivatization with trimethylsulfonium hydroxide (TMSH). Separation of two saturated (C13:0 and C15:0) and six unsaturated ginkgolic acid methyl esters with different positional double bonds (C15:1 Δ8 and Δ10, C17:1 Δ8, Δ10, and Δ12, and C17:2) was achieved on a very polar (88% cyanopropyl) aryl-polysiloxane HP-88 capillary GC column. The double bond positions in the GAs were determined by ozonolysis. The developed GC/MS method was validated according to ICH guidelines, and the quantitation results were verified by comparison with a standard high-performance liquid chromatography method. Nineteen G. biloba authenticated and commercial plant samples and 21 dietary supplements purported to contain G. biloba leaf extracts were analyzed. Finally, the presence of the marker compounds, terpene trilactones and flavonol glycosides for Ginkgo biloba in the dietary supplements was determined by UHPLC/MS and used to confirm the presence of G. biloba leaf extracts in all of the botanical dietary supplements.

Determination of fatty acid methyl esters derived from algae Scenedesmus dimorphus biomass by GC-MS with one-step esterification of free fatty acids and transesterification of glycerolipids.

PubMed

Avula, Satya Girish Chandra; Belovich, Joanne M; Xu, Yan

2017-05-01

Algae can synthesize, accumulate and store large amounts of lipids in its cells, which holds immense potential as a renewable source of biodiesel. In this work, we have developed and validated a GC-MS method for quantitation of fatty acids and glycerolipids in forms of fatty acid methyl esters derived from algae biomass. Algae Scenedesmus dimorphus dry mass was pulverized by mortar and pestle, then extracted by the modified Folch method and fractionated into free fatty acids and glycerolipids on aminopropyl solid-phase extraction cartridges. Fatty acid methyl esters were produced by an optimized one-step esterification of fatty acids and transesterification of glycerolipids with boron trichloride/methanol. The matrix effect, recoveries and stability of fatty acids and glycerolipids in algal matrix were first evaluated by spiking stable isotopes of pentadecanoic-2,2-d 2 acid and glyceryl tri(hexadecanoate-2,2-d 2 ) as surrogate analytes and tridecanoic-2,2-d 2 acid as internal standard into algal matrix prior to sample extraction. Later, the method was validated in terms of lower limits of quantitation, linear calibration ranges, intra- and inter-assay precision and accuracy using tridecanoic-2,2-d 2 acid as internal standard. The method developed has been applied to the quantitation of fatty acid methyl esters from free fatty acid and glycerolipid fractions of algae Scenedesmus dimorphus. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Development and validation of a method for the simultaneous extraction and separate measurement of oxytetracycline, florfenicol, oxolinic acid and flumequine from marine sediments.

PubMed

Norambuena, Luis; Gras, Nuri; Contreras, Sergio

2013-08-15

A simple and rapid method for the detection and extraction of oxolinic acid, flumequine, florfenicol and oxytetracycline from marine sediments was developed and validated. The analytes were extracted from the marine sediment using a solution of oxalic acid diluted in methanol with sonication before detection by HPLC using a diode-array detector (florfenicol and oxytetracycline) and fluorescence (oxolinic acid and flumequine). The quantification limits (QL) were 100 ng/g for oxytetracycline and florfenicol and 5 ng/g for oxolinic acid and flumequine. The coefficients of variation of the repeatability and intermediate precision were less than 10% in all of the analytes. The calibration curves were linear between 50 and 500 ng/ml for oxytetracycline and florfenicol and 1 and 20 ng/ml for oxolinic acid and flumequine. The recuperation rate for the analytes was above 86%. Copyright © 2013 Elsevier Ltd. All rights reserved.

Total lactic acid bacteria, antioxidant activity, and acceptance of synbiotic yoghurt with red ginger extract (Zingiberofficinale var. rubrum)

NASA Astrophysics Data System (ADS)

Larasati, B. A.; Panunggal, B.; Afifah, D. N.; Anjani, G.; Rustanti, N.

2018-02-01

Antioxidant related to oxidative stress can caused the metabolic disorders. A functional food that high in antioxidant can be use as the alternative prevention. The addition of red ginger extract in yoghurt could form a functional food, that high in antioxidant, synbiotic and fiber. The influence of red ginger extract on yoghurt synbiotic against lactic acid bacteria, antioxidant activity and acceptance were analyzed. This was an experimental research with one factor complete randomized design, specifically the addition of red ginger extract 0%; 0,1%; 0,3% and 0,5% into synbiotic yoghurt. Total plate count method used to analyze the lactic acid bacteria, 1-1-diphenyl-2-picrylhydrazyl (DPPH) method for antioxidant activity, and acceptance analyzed with hedonic test. The higher the dose of extract added to synbiotic yoghurt, the antioxidant activity got significantly increased (ρ=0,0001), while the lactic acid bacteria got insignificantly decreased (ρ=0,085). The addition of 0,5% red ginger extract obtained the antioxidant activity of 71% and 4,86 × 1013 CFU/ml on lactic acid bacteria, which the requirement for probiotic on National Standard of Indonesia is >107 CFU/ml. The addition of extract had a significant effect on acceptance (ρ=0,0001) in flavor, color, and texture, but not aroma (ρ=0,266). The optimal product in this research was the yoghurt synbiotic with addition of 0,1% red ginger extract. To summarize, the addition of red ginger extract in synbiotic yoghurt had significant effect on antioxidant activity, flavor, color, and texture, but no significant effect on lactic acid bacteria and aroma.

Comparison of supercritical fluid extraction and ultrasound-assisted extraction of fatty acids from quince (Cydonia oblonga Miller) seed using response surface methodology and central composite design.

PubMed

Daneshvand, Behnaz; Ara, Katayoun Mahdavi; Raofie, Farhad

2012-08-24

Fatty acids of Cydonia oblonga Miller cultivated in Iran were obtained by supercritical (carbon dioxide) extraction and ultrasound-assisted extraction methods. The oils were analyzed by capillary gas chromatography using mass spectrometric detections. The compounds were identified according to their retention indices and mass spectra (EI, 70eV). The experimental parameters of SFE such as pressure, temperature, modifier volume, static and dynamic extraction time were optimized using a Central Composite Design (CCD) after a 2(5) factorial design. Pressure and dynamic extraction time had significant effect on the extraction yield, while the other factors (temperature, static extraction time and modifier volume) were not identified as significant factors under the selected conditions. The results of chemometrics analysis showed the highest yield for SFE (24.32%), which was obtained at a pressure of 353bar, temperature of 35°C, modifier (methanol) volume of 150μL, and static and dynamic extraction times of 10 and 60min, respectively. Ultrasound-assisted extraction (UAE) of Fatty acids from C. oblonga Miller was optimized, using a rotatable central composite design. The optimum conditions were as follows: solvent (n-hexane) volume, 22mL; extraction time, 30min; and extraction temperature, 55°C. This resulted in a maximum oil recovery of 19.5%. The extracts with higher yield from both methods were subjected to transesterification and GC-MS analysis. The results show that the oil obtained by SFE with the optimal operating conditions allowed a fatty acid composition similar to the oil obtained by UAE in optimum condition and no significant differences were found. The major components of oil extract were Linoleic, Palmitic, Oleic, Stearic and Eicosanoic acids. Copyright © 2012 Elsevier B.V. All rights reserved.

Phytochemical Comparison of the Water and Ethanol Leaf Extracts of the Cree medicinal plant, Sarracenia purpurea L. (Sarraceniaceae).

PubMed

Cieniak, Carolina; Walshe-Roussel, Brendan; Liu, Rui; Muhammad, Asim; Saleem, Ammar; Haddad, Pierre S; Cuerrier, Alain; Foster, Brian C; Arnason, John T

2015-01-01

The Cree of Eeyou Istchee in Northern Quebec identified Sarracenia purpurea L. as an important plant for the treatment of Type 2 diabetes. Traditionally the plant is used as a decoction (boiling water extract) of the leaf, however, in order to study the extract in a laboratory setting, an 80% ethanol extract was used. In this study, the phytochemistry of both extracts of the leaves was compared and quantified. Two S. purpurea leaf extracts were prepared, one a traditional hot water extract and the other an 80% ethanol extract. Using UPLC-ESI-MS, the extracts were phytochemically compared for 2 triterpenes, betulinic acid and ursolic acid, using one gradient method and for 10 additional substances, including the actives quercetin-3-O-galactoside and morroniside, using a different method. The concentrations of the nine phenolic substances present, as well as an active principle, the iridoid glycoside morroniside, were very similar between the two extracts, with generally slightly higher concentrations of phenolics in the ethanol extract as expected. However, two triterpenes, betulinic acid and ursolic acid, were 107 and 93 times more concentrated, respectively, in the ethanol extract compared to the water extract. The main phytochemical markers and most importantly the antidiabetic active principles, quercetin-3-O-galactoside and morroniside, were present in similar amounts in the two extracts, which predicts similar bioactivity.This article is open to POST-PUBLICATION REVIEW. Registered readers (see "For Readers") may comment by clicking on ABSTRACT on the issue's contents page.

Phenolic content and antioxidant properties of seeds from different grape cultivars grown in Iran.

PubMed

Mirbagheri, Vasigheh Sadat; Alizadeh, Ebrahim; Yousef Elahi, Mostafa; Esmaeilzadeh Bahabadi, Sedigheh

2018-02-01

This study investigated the antioxidant activity and phenolic composition of seed extracts from three grape cultivars grown in Iran. Folin Ciocalteu method was used for the determination of the total phenolic contents and GC-MS was used for the analysis of phenolic compositions. 1,1-diphenyl-2-picrylhydrazyl (DPPH) method was used to evaluate the antioxidant activity. The highest and the lowest total phenolic contents of seed extract were found in the black and green grape, respectively. The content of individual phenols such as Frulic acid, Gentistic acid, Syringic acid, (+) Catechin, Chlorogenic acid and (-)- Epicatchin gallate was cultivars dependent. The antioxidant activity of the seed extracts ranged from 34.03% (Green) to 53.63% (Black). Generally, the Black grape seed extract with the total phenolic content (3 ± 0.01 mg tannic acid/g DM), DPPH (53.63 ± 0.34%), IC 50 and AEAC (7.41 and 16.92 mg/mL) showed the highest level of total antioxidant capacity.

Evaluation of antimicrobial activity of extracts of Tibouchina candolleana (melastomataceae), isolated compounds and semi-synthetic derivatives against endodontic bacteria.

PubMed

Dos Santos, Fernanda M; de Souza, Maria Gorete; Crotti, Antônio E Miller; Martins, Carlos H G; Ambrósio, Sérgio R; Veneziani, Rodrigo C S; E Silva, Márcio L Andrade; Cunha, Wilson R

2012-04-01

This work describes the phytochemical study of the extracts from aerial parts of Tibouchina candolleana as well as the evaluation of the antimicrobial activity of extracts, isolated compounds, and semi-synthetic derivatives of ursolic acid against endodontic bacteria. HRGC analysis of the n-hexane extract of T. candolleana allowed identification of β-amyrin, α-amyrin, and β-sitosterol as major constituents. The triterpenes ursolic acid and oleanolic acid were isolated from the methylene chloride extract and identified. In addition, the flavonoids luteolin and genistein were isolated from the ethanol extract and identified. The antimicrobial activity was investigated via determination of the minimum inhibitory concentration (MIC) using the broth microdilution method. Amongst the isolated compounds, ursolic acid was the most effective against the selected endodontic bacteria. As for the semi-synthetic ursolic acid derivatives, only the methyl ester derivative potentiated the activity against Bacteroides fragilis.

Evaluation of antimicrobial activity of extracts of Tibouchina candolleana (melastomataceae), isolated compounds and semi-synthetic derivatives against endodontic bacteria

PubMed Central

dos Santos, Fernanda M.; de Souza, Maria Gorete; Crotti, Antônio E. Miller; Martins, Carlos H. G.; Ambrósio, Sérgio R.; Veneziani, Rodrigo C. S.; e Silva, Márcio L. Andrade; Cunha, Wilson R.

2012-01-01

This work describes the phytochemical study of the extracts from aerial parts of Tibouchina candolleana as well as the evaluation of the antimicrobial activity of extracts, isolated compounds, and semi-synthetic derivatives of ursolic acid against endodontic bacteria. HRGC analysis of the n-hexane extract of T. candolleana allowed identification of β-amyrin, α-amyrin, and β-sitosterol as major constituents. The triterpenes ursolic acid and oleanolic acid were isolated from the methylene chloride extract and identified. In addition, the flavonoids luteolin and genistein were isolated from the ethanol extract and identified. The antimicrobial activity was investigated via determination of the minimum inhibitory concentration (MIC) using the broth microdilution method. Amongst the isolated compounds, ursolic acid was the most effective against the selected endodontic bacteria. As for the semi-synthetic ursolic acid derivatives, only the methyl ester derivative potentiated the activity against Bacteroides fragilis. PMID:24031892

Evaluation of spectrophotometric and HPLC methods for shikimic acid determination in plants: models in glyphosate-resistant and -susceptible crops.

PubMed

Zelaya, Ian A; Anderson, Jennifer A H; Owen, Micheal D K; Landes, Reid D

2011-03-23

Endogenous shikimic acid determinations are routinely used to assess the efficacy of glyphosate in plants. Numerous analytical methods exist in the public domain for the detection of shikimic acid, yet the most commonly cited comprise spectrophotometric and high-pressure liquid chromatography (HPLC) methods. This paper compares an HPLC and two spectrophotometric methods (Spec 1 and Spec 2) and assesses the effectiveness in the detection of shikimic acid in the tissues of glyphosate-treated plants. Furthermore, the study evaluates the versatility of two acid-based shikimic acid extraction methods and assesses the longevity of plant extract samples under different storage conditions. Finally, Spec 1 and Spec 2 are further characterized with respect to (1) the capacity to discern between shikimic acid and chemically related alicyclic hydroxy acids, (2) the stability of the chromophore (t1/2), (3) the detection limits, and (4) the cost and simplicity of undertaking the analytical procedure. Overall, spectrophotometric methods were more cost-effective and simpler to execute yet provided a narrower detection limit compared to HPLC. All three methods were specific to shikimic acid and detected the compound in the tissues of glyphosate-susceptible crops, increasing exponentially in concentration within 24 h of glyphosate application and plateauing at approximately 72 h. Spec 1 estimated more shikimic acid in identical plant extract samples compared to Spec 2 and, likewise, HPLC detection was more effective than spectrophotometric determinations. Given the unprecedented global adoption of glyphosate-resistant crops and concomitant use of glyphosate, an effective and accurate assessment of glyphosate efficacy is important. Endogenous shikimic acid determinations are instrumental in corroborating the efficacy of glyphosate and therefore have numerous applications in herbicide research and related areas of science as well as resolving many commercial issues as a consequence of glyphosate utilization.

[Research of the essential oil of Plumeria rubra var. actifolia from Laos by supercritical carbon dioxide extraction].

PubMed

Xiao, Xin-Yu; Cui, Long-Hai; Zhou, Xin-Xin; Wu, Yan; Ge, Fa-Huan

2011-05-01

The orthogonal test and the supercritical carbon dioxide fluid extraction were used for optimizing the extraction of the essential oil from Plumeria rubra var. actifolia for the first time. Compared with the steam distillation, the optimal operation parameter of extraction was as follows: extraction pressure 25 MPa, extraction temperature 45 degrees C; separator I pressure 12 MPa, separator I temperature 55 degrees C; separator II pressure 6 MPa, separator II temperature 30 degrees C. Under this condition the yield of the essential oil was 5.8927%. The components were separated and identified by GC-MS. 53 components of Plumeria rubra var. actifolia measured by SFE method were identified and determined by normalization method. The main components were 1, 6, 10-dodecatrien-3-ol, 3, 7, 11-trimethyl, benzoic acid, 2-hydroxy-, phenylmethyl ester, 1, 2-benzenedicarboxylic acid, bis(2-methylpropyl) ester,etc.. 1, 2-Benzenedicarboxylic acid, bis (2-methylpropyl) este. took up 66.11% of the total amount, and there was much difference of the results from SD method.

Quantitative determination of acidic hydrolysis products of Chemical Weapons Convention related chemicals from aqueous and soil samples using ion-pair solid-phase extraction and in situ butylation.

PubMed

Pal Anagoni, Suresh; Kauser, Asma; Maity, Gopal; Upadhyayula, Vijayasarathi V R

2018-02-01

Chemical warfare agents such as organophosphorus nerve agents, mustard agents, and psychotomimetic agent like 3-quinuclidinylbenzilate degrade in the environment and form acidic degradation products, the analysis of which is difficult under normal analytical conditions. In the present work, a simultaneous extraction and derivatization method in which the analytes are butylated followed by gas chromatography and mass spectrometric identification of the analytes from aqueous and soil samples was carried out. The extraction was carried out using ion-pair solid-phase extraction with tetrabutylammonium hydroxide followed by gas chromatography with mass spectrometry in the electron ionization mode. Various parameters such as optimum concentration of the ion-pair reagent, pH of the sample, extraction solvent, and type of ion-pair reagent were optimized. The method was validated for various parameters such as linearity, accuracy, precision, and limit of detection and quantification. The method was observed to be linear from 1 to 1000 ng/mL range in selected ion monitoring mode. The extraction recoveries were in the range of 85-110% from the matrixes with the limit of quantification for alkyl phosphonic acids at 1 ng/mL, thiodiglycolic acid at 20 ng/mL, and benzilic acid at 50 ng/mL with intra- and interday precisions below 15%. The developed method was applied for the samples prepared in the scenario of challenging inspection. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Evaluation, prediction and optimization the ultrasound-assisted extraction method using response surface methodology: antioxidant and biological properties of Stachys parviflora L.

PubMed Central

Bashi, Davoud Salar; Dowom, Samaneh Attaran; Bazzaz, Bibi Sedigheh Fazly; Khanzadeh, Farhad; Soheili, Vahid; Mohammadpour, Ali

2016-01-01

Objective(s): To optimize the extraction method using response surface methodology, extract the phenolic compounds, and identify the antioxidant and biological properties of Stachys parviflora L. extracts. Materials and Methods: Maceration and ultrasound-assisted extraction (UAE) (4, 7, 10 min treatment time, 40, 70, 100 % high-intensity and 60, 80, 100 % (v v-1) methanol purity) were applied to obtain the extracts. SEM was conducted to provide the microstructure of the extracted plant. MICs (colorimetric assay), MFCs (colony diameter), total phenolic content, total flavonoid content, radical scavenging capacity and extraction efficiency were determined. HPLC analysis was applied to measure the existent phenolic compounds. Results: A quadratic model (4 min treatment time, 74.5 % high-intensity and 74.2 % solvent purity) was suggested as the best (TPC: 20.89 mg GAE g-1 d.m., TFC: 6.22 mg QEs g-1 d.m., DPPH IC50: 21.86 µg ml-1 and EE: 113.65 mg g-1 d.m.) UAE extraction model. The optimized UAE extract was generally more effective against Gram-positive microorganisms (MIC: 10-20; MBC: 10-40 (mg ml-1)) than Gram-negative ones (MIC: 40; MBC: >40 (mg ml-1)). Moreover, it (MGI: 2.32-100 %) revealed more anti-mold activity than maceration (MGI: <28.77 %). Explosive disruption of the cell walls, therefore, enhanced extraction yield by acoustic cavitation, was elucidated using SEM. Caffeic acid, tannic acid, quercetin, trans ferulic acid and rosmarinic acid were determined as the phenolic compounds in the optimized extract. Conclusion: RSM optimization was successfully applied for UAE from S. parviflora. The considerable antioxidant and biological properties were attributed to the phenolic compounds. PMID:27403260

Simultaneous determination of docosahexaenoic acid and eicosapentaenoic acid in common seafood using ultrasonic cell crusher extraction combined with gas chromatography.

PubMed

Zhao, Juanjuan; Ren, Yan; Yu, Chen; Chen, Xiangming; Shi, Yanan

2017-02-01

An effective method for the simultaneous determination of docosahexaenoic acid and eicosapentaenoic acid in common seafood by gas chromatography was developed and validated. Total docosahexaenoic acid and eicosapentaenoic acid were extracted from seafood by ultrasonic cell crusher assisted extraction and methyl esterified for gas chromatography analysis in the presence of the internal standard. The linearity was good (r > 0.999) in 9.59 ∼ 479.5 μg/mL for docosahexaenoic acid and 9.56 ∼ 477.8 μg/mL for eicosapentaenoic acid. The intrarun and interrun precisions were both within 4.8 and 6.1% for the two analytes, while the accuracy was less than 5.8%. The developed method was applied for determination of docosahexaenoic acid and eicosapentaenoic acid in six kinds of seafood. The result showed the content of docosahexaenoic acid and eicosapentaenoic acid was all higher than 1 mg/g in yellow croaker, hairtail, venerupis philippinarum, mussel, and oyster. Our work may be helpful for dietary optimization and production of docosahexaenoic acid and eicosapentaenoic acid. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Virus inactivation by nucleic acid extraction reagents.

PubMed

Blow, Jamie A; Dohm, David J; Negley, Diane L; Mores, Christopher N

2004-08-01

Many assume that common methods to extract viral nucleic acids are able to render a sample non-infectious. It may be that inactivation of infectious virus is incomplete during viral nucleic acid extraction methods. Accordingly, two common viral nucleic acid extraction techniques were evaluated for the ability to inactivate high viral titer specimens. In particular, the potential for TRIzol LS Reagent (Invitrogen Corp., Carlsbad, CA) and AVL Buffer (Qiagen, Valencia, CA) were examined to render suspensions of alphaviruses, flaviviruses, filoviruses and a bunyavirus non-infectious to tissue culture assay. The dilution series for both extraction reagents consistently caused cell death through a 100-fold dilution. Except for the DEN subtype 4 positive control, all viruses had titers of at least 10(6)pfu/ml. No plaques were detected in any extraction reagent plus virus combination in this study, therefore, the extraction reagents appeared to inactivate completely each of the high-titer viruses used in this study. These results support the reliance upon either TRIzol LS Reagent or AVL Buffer to render clinical or environmental samples non-infectious, which has implications for the handling and processing of samples under austere field conditions and low level containment.

Improved tandem mass spectrometry (MS/MS) derivatized method for the detection of tyrosinemia type I, amino acids and acylcarnitine disorders using a single extraction process.

PubMed

Dhillon, Kuldeep S; Bhandal, Ajit S; Aznar, Constantino P; Lorey, Fred W; Neogi, Partha

2011-05-12

Succinylacetone (SUAC), a specific marker for tyrosinemia type I (Tyr I) cannot be detected by the routine LC-MS/MS screening of amino acids (AA) and acylcarnitines (AC) in newborns. The current derivatized methods require double extraction of newborn dried blood spots (DBS); one for AA and AC and the second for SUAC from the blood spot left after the first extraction. We have developed a method in which AA, AC and SUAC are extracted in a single extraction resulting in significant reduction in labor and assay time. The 3.2 mm DBS were extracted by incubating at 45 °C for 45 min with 100 μl of acetonitrile (ACN)-water-formic acid mixture containing hydrazine and stable-isotope labeled internal standards of AA, AC and SUAC. The extract was derivatized with n-butanolic-HCl and analyzed by LC-MS/MS. The average inter-assay CVs for, AA, AC and SUAC were 10.1, 10.8 and 7.1% respectively. The extraction of analytes with ACN-water mixture showed no significant difference in their recovery compared to commonly used solvent MeOH. The concentration of hydrazine had considerable impact on SUAC extraction. We developed a new MS/MS derivatized method to detect AA/AC/SUAC in a single extraction process for screening Tyr I along with disorders of AA and AC. Published by Elsevier B.V.

A study of extraction process and in vitro antioxidant activity of total phenols from Rhizoma Imperatae.

PubMed

Zhou, Xian-rong; Wang, Jian-hua; Jiang, Bo; Shang, Jin; Zhao, Chang-qiong

2013-01-01

The study investigated the extraction method of Rhizoma Imperatae and its antioxidant activity, and provided a basis for its rational development. The extraction method of Rhizoma Imperatae was determined using orthogonal design test and by total phenol content, its hydroxyl radical scavenging ability was measured by Fenton reaction, and potassium ferricyanide reduction method was used to determine its reducing power. The results showed that the optimum extraction process of Rhizoma Imperatae was a 50-fold volume of water, 30 °C, three times of extraction with 2 h each. Its IC50 for scavenging of hydroxyl radicals was 0.0948 mg/mL, while IC50 of ascorbic acid was 0.1096 mg/mL; in the ferricyanide considerable reduction method, the extract exhibited reducing power comparable to that of the ascorbic acid. The study concluded that Rhizoma Imperatae extract contains relatively large amount of polyphenols, and has a good anti-oxidation ability.

Green Extraction of Natural Antioxidants from the Sterculia nobilis Fruit Waste and Analysis of Phenolic Profile.

PubMed

Zhang, Jiao-Jiao; Li, Ya; Lin, Sheng-Jun; Li, Hua-Bin

2018-05-02

The waste of Sterculia nobilis fruit was massively produced during food processing, which contains lots of natural antioxidants. In this study, antioxidants in the Sterculia nobilis fruit waste were extracted using the green microwave-assisted extraction (MAE) technique. The effects of five independent variables (ethanol concentration, solvent/material ratio, extraction time, temperature, and microwave power) on extraction efficiency were explored, and three major factors (ethanol concentration, extraction time, and temperature) showing great influences were chosen to study their interactions by response surface methodology. The optimal conditions were as follows: 40.96% ethanol concentration, 30 mL/g solvent/material ratio, 37.37 min extraction time at 66.76 °C, and 700 W microwave power. The Trolox equivalent antioxidant capacity value obtained in optimal conditions was in agreement with the predicted value. Besides, MAE improved the extraction efficiency compared with maceration and Soxhlet extraction methods. Additionally, the phenolic profile in the extract was analyzed by UPLC-MS/MS, and eight kinds of phenolic compounds were identified and quantified, including epicatechin, protocatechuic acid, ferulic acid, gallic acid, p -coumaric acid, caffeic acid, quercetin, and p -hydroxycinnamic acid. This study could contribute to the value-added utilization of the waste from Sterculia nobilis fruit, and the extract could be developed as food additive or functional food.

Chromatographic and mass spectrometric characterization of essential oils and extracts from Lippia (Verbenaceae) aromatic plants.

PubMed

Stashenko, Elena E; Martínez, Jairo R; Cala, Mónica P; Durán, Diego C; Caballero, Deyanira

2013-01-01

Analytical methodologies based on GC and HPLC were developed for the separation and quantification of carnosic acid, ursolic acid, caffeic acid, p-coumaric acid, rosmarinic acid, apigenin, luteolin, quercetin, kaempferol, naringenin, and pinocembrin. These methods were used to characterize essential oils and extracts obtained by solvent (methanol) and by supercritical fluid (CO(2)) extraction from stems and leaves of Lippia (Verbenaceae family) aromatic plants (Lippia alba, Lippia origanoides, Lippia micromera, Lippia americana, Lippia graveolens, and Lippia citriodora). Supercritical CO(2) extraction isolated solely pinocembrin and narigenin from three L. origanoides chemotypes. Solvent extracts possessed a more varied composition that additionally included apigenin, quercetin, and luteolin. Solvent extraction afforded higher overall flavonoid yields from all species in comparison with supercritical CO(2) extraction. Pinocembrin was determined in L. origanoides extract at a concentration of 30 mg/g of plant material, which is more than ten times higher than the amount at which polyphenols are regularly found in aromatic plant extracts. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction of metals using supercritical fluid and chelate forming legand

DOEpatents

Wai, Chien M.; Laintz, Kenneth E.

1998-01-01

A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a supercritical fluid solvent containing a chelating agent is described. The chelating agent forms chelates that are soluble in the supercritical fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is a fluorinated .beta.-diketone. In especially preferred embodiments the extraction solvent is supercritical carbon dioxide, and the chelating agent comprises a fluorinated .beta.-diketone and a trialkyl phosphate, or a fluorinated .beta.-diketone and a trialkylphosphine oxide. Although a trialkyl phosphate can extract lanthanides and actinides from acidic solutions, a binary mixture comprising a fluorinated .beta.-diketone and a trialkyl phosphate or a trialkylphosphine oxide tends to enhance the extraction efficiencies for actinides and lanthanides. The method provides an environmentally benign process for removing contaminants from industrial waste without using acids or biologically harmful solvents. The method is particularly useful for extracting actinides and lanthanides from acidic solutions. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

Extraction of metals using supercritical fluid and chelate forming ligand

DOEpatents

Wai, C.M.; Laintz, K.E.

1998-03-24

A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a supercritical fluid solvent containing a chelating agent is described. The chelating agent forms chelates that are soluble in the supercritical fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is a fluorinated {beta}-diketone. In especially preferred embodiments the extraction solvent is supercritical carbon dioxide, and the chelating agent comprises a fluorinated {beta}-diketone and a trialkyl phosphate, or a fluorinated {beta}-diketone and a trialkylphosphine oxide. Although a trialkyl phosphate can extract lanthanides and actinides from acidic solutions, a binary mixture comprising a fluorinated {beta}-diketone and a trialkyl phosphate or a trialkylphosphine oxide tends to enhance the extraction efficiencies for actinides and lanthanides. The method provides an environmentally benign process for removing contaminants from industrial waste without using acids or biologically harmful solvents. The method is particularly useful for extracting actinides and lanthanides from acidic solutions. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process. 7 figs.

An efficient chemical analysis of phenolic acids and flavonoids in raw propolis by microwave-assisted extraction combined with high-performance liquid chromatography using the fused-core technology.

PubMed

Pellati, Federica; Prencipe, Francesco Pio; Bertelli, Davide; Benvenuti, Stefania

2013-01-01

A closed-vessel microwave-assisted extraction (MAE) technique was optimized for the first time for the extraction of polyphenols from raw propolis. The results obtained by means of response surface experimental design methodology showed that the best global response was reached when the extraction temperature was set at 106 °C, the solvent composition close to EtOH-H2O 80:20 (v/v), with an extraction time of 15 min. In comparison with other techniques, such as maceration, heat reflux extraction (HRE) and ultrasound-assisted extraction (UAE), the extraction with MAE was improved by shorter extraction time and lower volume of solvent needed. The HPLC analyses of propolis extracts were carried out on a fused-core Ascentis Express C18 column (150 mm × 3.0 mm I.D., 2.7 μm), with a gradient mobile phase composed by 0.1% formic acid in water and acetonitrile. Detection was performed by DAD and MS. The method validation indicated that the correlation coefficients were >0.999; the limit of detection was in the range 0.5-0.8 μg/ml for phenolic acids and 1.2-3.0 μg/ml for flavonoids; the recovery range was 95.3-98.1% for phenolic acids and 94.1-101.3% for flavonoids; the intra- and inter-day %RSD values for retention times and peak areas were ≤ 0.3 and 2.2%, respectively. The quali- and quantitative analysis of polyphenols in Italian samples of raw propolis was performed with the validated method. Total phenolic acids ranged from 5.0 to 120.8 mg/g and total flavonoids from 2.5 to 168.0mg/g. The proposed MAE procedure and HPLC method can be considered reliable and useful tools for the comprehensive multi-component analysis of polyphenols in propolis extracts to be used in apitherapy. Copyright © 2013 Elsevier B.V. All rights reserved.

Stability Test and Quantitative and Qualitative Analyses of the Amino Acids in Pharmacopuncture Extracted from Scolopendra subspinipes mutilans.

PubMed

Cho, GyeYoon; Han, KyuChul; Yoon, JinYoung

2015-03-01

Scolopendra subspinipes mutilans (S. subspinipes mutilans) is known as a traditional medicine and includes various amino acids, peptides and proteins. The amino acids in the pharmacopuncture extracted from S. subspinipes mutilans by using derivatization methods were analyzed quantitatively and qualitatively by using high performance liquid chromatography (HPLC) over a 12 month period to confirm its stability. Amino acids of pharmacopuncture extracted from S. subspinipes mutilans were derived by using O-phthaldialdehyde (OPA) & 9-fluorenyl methoxy carbonyl chloride (FMOC) reagent and were analyzed using HPLC. The amino acids were detected by using a diode array detector (DAD) and a fluorescence detector (FLD) to compare a mixed amino acid standard (STD) to the pharmacopuncture from centipedes. The stability tests on the pharmacopuncture from centipedes were done using HPLC for three conditions: a room temperature test chamber, an acceleration test chamber, and a cold test chamber. The pharmacopuncture from centipedes was prepared by using the method of the Korean Pharmacopuncture Institute (KPI) and through quantitative analyses was shown to contain 9 amino acids of the 16 amino acids in the mixed amino acid STD. The amounts of the amino acids in the pharmacopuncture from centipedes were 34.37 ppm of aspartate, 123.72 ppm of arginine, 170.63 ppm of alanine, 59.55 ppm of leucine and 57 ppm of lysine. The relative standard deviation (RSD %) results for the pharmacopuncture from centipedes had a maximum value of 14.95% and minimum value of 1.795% on the room temperature test chamber, the acceleration test chamber and the cold test chamber stability tests. Stability tests on and quantitative and qualitative analyses of the amino acids in the pharmacopuncture extracted from centipedes by using derivatization methods were performed by using HPLC. Through research, we hope to determine the relationship between time and the concentrations of the amino acids in the pharmacopuncture extracted from centipedes.

The fluorimetric microdetermination of glyoxylic acid in blood, urine and bacterial extracts

PubMed Central

Zarembski, P. M.; Hodgkinson, A.

1965-01-01

1. A spectrophotofluorimetric method for the determination of glyoxylic acid in biological materials is described. 2. The method is based on the reaction between glyoxylic acid and resorcinol in acid solution, a fluorescent complex being obtained on the subsequent addition of alkali. 3. The reaction was found to be sensitive and highly specific, the minimum detectable amount of glyoxylic acid being 1·35×10−8 mole. 4. The urinary excretion of glyoxylic acid by ten normal adults ranged from 1·4 to 4·7mg./24hr. Small but measurable amounts of glyoxylic acid were found in cell-free extracts of Pseudomonas oxalaticus OX1 grown on oxalic acid as a source of carbon. No glyoxylic acid was detected in human serum. PMID:14343135

Development of a method for the quantitation of chloro-, bromo-, and iodoacetic acids in alcoholic beverages.

PubMed

Cardador, Maria Jose; Gallego, Mercedes

2012-01-25

Chloroacetic, bromoacetic, and iodoacetic acids can be found in alcoholic beverages when they are used as preservatives/stabilizers or as disinfectants. As they are toxic components, their addition is not permitted under European Union and U.S. regulations. To date, no sensitive methods are available, and those proposed are very laborious. This paper describes a sensitive and straightforward method for the determination of the three monohalogenated acetic acids (m-HAAs) in wines and beers using static headspace extraction coupled with gas chromatography-mass spectrometry. Prior to extraction, the target analytes were esterified to increase their volatility, and all parameters related to the extraction/methylation process were optimized to achieve high efficiency (>90%). The study examined the influence both of the ethanol concentration on the headspace partitioning and of the primary acids present in wine on the derivatization reaction of the m-HAAs. The proposed method allows the determination of these compounds at microgram per liter levels in alcoholic beverages.

Arsenic Speciation and Extraction and the Significance of Biodegradable Acid on Arsenic Removal—An Approach for Remediation of Arsenic-Contaminated Soil

PubMed Central

Nguyen Van, Thinh; Osanai, Yasuhito; Do Nguyen, Hai; Kurosawa, Kiyoshi

2017-01-01

A series of arsenic remediation tests were conducted using a washing method with biodegradable organic acids, including oxalic, citric and ascorbic acids. Approximately 80% of the arsenic in one sample was removed under the effect of the ascorbic and oxalic acid combination, which was roughly twice higher than the effectiveness of the ascorbic and citric acid combination under the same conditions. The soils treated using biodegradable acids had low remaining concentrations of arsenic that are primarily contained in the crystalline iron oxides and organic matter fractions. The close correlation between extracted arsenic and extracted iron/aluminum suggested that arsenic was removed via the dissolution of Fe/Al oxides in soils. The fractionation of arsenic in four contaminated soils was investigated using a modified sequential extraction method. Regarding fractionation, we found that most of the soil contained high proportions of arsenic (As) in exchangeable fractions with phosphorus, amorphous oxides, and crystalline iron oxides, while a small amount of the arsenic fraction was organic matter-bound. This study indicated that biodegradable organic acids can be considered as a means for arsenic-contaminated soil remediation.

Simultaneous Determination of Oleanolic Acid and Ursolic Acid by in Vivo Microdialysis via UHPLC-MS/MS Using Magnetic Dispersive Solid Phase Extraction Coupling with Microwave-Assisted Derivatization and Its Application to a Pharmacokinetic Study of Arctiumlappa L. Root Extract in Rats.

PubMed

Zheng, Zhenjia; Zhao, Xian-En; Zhu, Shuyun; Dang, Jun; Qiao, Xuguang; Qiu, Zhichang; Tao, Yanduo

2018-04-18

Simultaneous detection of oleanolic acid and ursolic acid in rat blood by in vivo microdialysis can provide important pharmacokinetics information. Microwave-assisted derivatization coupled with magnetic dispersive solid phase extraction was established for the determination of oleanolic acid and ursolic acid by liquid chromatography tandem mass spectrometry. 2'-Carbonyl-piperazine rhodamine B was first designed and synthesized as the derivatization reagent, which was easily adsorbed onto the surface of Fe 3 O 4 /graphene oxide. Simultaneous derivatization and extraction of oleanolic acid and ursolic acid were performed on Fe 3 O 4 /graphene oxide. The permanent positive charge of the derivatization reagent significantly improved the ionization efficiencies. The limits of detection were 0.025 and 0.020 ng/mL for oleanolic acid and ursolic acid, respectively. The validated method was shown to be promising for sensitive, accurate, and simultaneous determination of oleanolic acid and ursolic acid. It was used for their pharmacokinetics study in rat blood after oral administration of Arctiumlappa L. root extract.

Predicting nucleic acid binding interfaces from structural models of proteins.

PubMed

Dror, Iris; Shazman, Shula; Mukherjee, Srayanta; Zhang, Yang; Glaser, Fabian; Mandel-Gutfreund, Yael

2012-02-01

The function of DNA- and RNA-binding proteins can be inferred from the characterization and accurate prediction of their binding interfaces. However, the main pitfall of various structure-based methods for predicting nucleic acid binding function is that they are all limited to a relatively small number of proteins for which high-resolution three-dimensional structures are available. In this study, we developed a pipeline for extracting functional electrostatic patches from surfaces of protein structural models, obtained using the I-TASSER protein structure predictor. The largest positive patches are extracted from the protein surface using the patchfinder algorithm. We show that functional electrostatic patches extracted from an ensemble of structural models highly overlap the patches extracted from high-resolution structures. Furthermore, by testing our pipeline on a set of 55 known nucleic acid binding proteins for which I-TASSER produces high-quality models, we show that the method accurately identifies the nucleic acids binding interface on structural models of proteins. Employing a combined patch approach we show that patches extracted from an ensemble of models better predicts the real nucleic acid binding interfaces compared with patches extracted from independent models. Overall, these results suggest that combining information from a collection of low-resolution structural models could be a valuable approach for functional annotation. We suggest that our method will be further applicable for predicting other functional surfaces of proteins with unknown structure. Copyright © 2011 Wiley Periodicals, Inc.

Development of an efficient fungal DNA extraction method to be used in random amplified polymorphic DNA-PCR analysis to differentiate cyclopiazonic acid mold producers.

PubMed

Sánchez, Beatriz; Rodríguez, Mar; Casado, Eva M; Martín, Alberto; Córdoba, Juan J

2008-12-01

A variety of previously established mechanical and chemical treatments to achieve fungal cell lysis combined with a semiautomatic system operated by a vacuum pump were tested to obtain DNA extract to be directly used in randomly amplified polymorphic DNA (RAPD)-PCR to differentiate cyclopiazonic acid-producing and -nonproducing mold strains. A DNA extraction method that includes digestion with proteinase K and lyticase prior to using a mortar and pestle grinding and a semiautomatic vacuum system yielded DNA of high quality in all the fungal strains and species tested, at concentrations ranging from 17 to 89 ng/microl in 150 microl of the final DNA extract. Two microliters of DNA extracted with this method was directly used for RAPD-PCR using primer (GACA)4. Reproducible RAPD fingerprints showing high differences between producer and nonproducer strains were observed. These differences in the RAPD patterns did not differentiate all the strains tested in clusters by cyclopiazonic acid production but may be very useful to distinguish cyclopiazonic acid producer strains from nonproducer strains by a simple RAPD analysis. Thus, the DNA extracts obtained could be used directly without previous purification and quantification for RAPD analysis to differentiate cyclopiazonic acid producer from nonproducer mold strains. This combined analysis could be adaptable to other toxigenic fungal species to enable differentiation of toxigenic and non-toxigenic molds, a procedure of great interest in food safety.

An alternative method to remove PEO-PPO-PEO template in organic-inorganic mesoporous nanocomposites by sulfuric acid extraction

NASA Astrophysics Data System (ADS)

Zhuang, Xin; Qian, Xufang; Lv, Jiahui; Wan, Ying

2010-06-01

Sulfuric acid is used as an extraction agent to remove PEO-PPO-PEO templates in the organic-inorganic mesoporous nanocomposites from the triconstituent co-assembly which includes the low-polymerized phenolic resins, TEOS and triblock copolymer F127. The XRD and TEM results show well ordered mesostructure after extraction with sulfuric acid. As followed from the N 2 sorption isotherms the extracted composites possess high surface areas (332-367 m 2/g), large pore volumes (0.66-0.78 cm 3/g), and large pore sizes (about 10.7 nm). The FT-IR analysis reveals almost complete elimination of triblock copolymer F127, and the maintenance of organic groups. This method shows potentials in removing templates from nanocomposites containing functional moieties.

Effects of microwave power and irradiation time on pectin extraction from watermelon rinds (Citrullus lanatus) with acetic acid using microwave assisted extraction method

NASA Astrophysics Data System (ADS)

Sari, A. M.; Ishartani, D.; Dewanty, P. S.

2018-01-01

The aims of this research are to study the effect of microwave power (119.7 W, 199.5 W and 279.3 W) and irradiation time (6, 9 and 12 min) on pectin extraction by using Microwave Assisted Extraction (MAE) with acetic acid and to do a preliminary characterization of pectin from watermelon rinds. A randomized factorial design with two factors was used to determine the effect of microwave power and processing time on the yield, equivalent weight, degree of methoxylation (DM), galacturonic acid content (GA) and the degree of esterification (DE) of extracted pectin. The results showed that extracted pectin from watermelon rinds using MAE method have yield ranged from 3.925% to 5.766%, with equivalent weight ranged from 1249.702 to 2007.756. Extracted pectin have a DM value ranged from 3.89% to 10.81%. Galacturonic acid content that meets with IPPA standard resulted from extraction condition of 279.3-watt microwave power for 9 min and 12 min. The degree of esterification (DE) value ranged from 56.86% to 85.76%, and this value exhibited a relatively high methoxyl pectin (>50%). The best pectin properties was obtained at a microwave power of 279.3 watts for 12 min.

Selective extraction of derivates of p-hydroxy-benzoic acid from plant material by using a molecularly imprinted polymer.

PubMed

Karasová, Gabriela; Lehotay, Jozef; Sádecká, Jana; Skacáni, Ivan; Lachová, Miroslava

2005-12-01

Selective SPE of derivates of p-hydroxybenzoic acid (pHBA) from plant extract of Melissa officinalis is presented using a molecularly imprinted polymer (MIP) made with protocatechuic acid (PA) as template molecule. MIP was prepared with acrylamide as functional monomer, ethylene glycol dimethacrylate as crosslinking monomer and ACN as porogen. MIP was evaluated towards six phenolic acids: PA, gallic acid, pHBA, vanillic acid (VA), gentisic acid (GeA) and syringic acid (SyrA), and then steps of molecularly imprinted SPE (MISPE) procedure were optimized. The best specific binding capacity of MIP was obtained for PA in ACN (34.7 microg/g of MIP). Other tested acids were also bound on MIP if they were dissolved in this solvent. ACN was chosen as solvent for sample application. M. officinalis was extracted into methanol/water (4:1, v/v), the extract was then evaporated to dryness and dissolved in ACN before application on MIP. Water and ACN were used as washing solvents and elution of benzoic acids was performed by means of a mixture methanol/acetic acid (9:1, v/v). pHBA, GA, PA and VA were extracted with recoveries of 56.3-82.1% using this MISPE method. GeA was not determined in plant extract.

Enhanced and green extraction polyphenols and furanocoumarins from Fig (Ficus carica L.) leaves using deep eutectic solvents.

PubMed

Wang, Tong; Jiao, Jiao; Gai, Qing-Yan; Wang, Peng; Guo, Na; Niu, Li-Li; Fu, Yu-Jie

2017-10-25

Nowadays, green extraction of bioactive compounds from medicinal plants has gained increasing attention. As green solvent, deep eutectic solvent (DES) have been highly rated to replace toxic organic solvents in extraction process. In present study, to simultaneous extraction five main bioactive compounds from fig leaves, DES was tailor-made. The tailor-made DES composed of a 3:3:3 molar ratio of glycerol, xylitol and D-(-)-Fructose showed enhanced extraction yields for five target compounds simultaneously compared with traditional methanol and non-tailor DESs. Then, the tailor-made DES based extraction methods have compared and microwave-assisted extraction was selected and optimized due to its high extraction yields with lower time consumption. The influencing parameters including extraction temperature, liquid-solid ratio, and extraction time were optimized using response surface methodology (RSM). Under optimal conditions the extraction yield of caffeoylmalic acid, psoralic acid-glucoside, rutin, psoralen and bergapten was 6.482mg/g, 16.34mg/g, 5.207mg/g, 15.22mg/g and 2.475mg/g, respectively. Macroporous resin D101 has been used to recovery target compounds with recovery yields of 79.2%, 83.4%, 85.5%, 81.2% and 75.3% for caffeoylmalic acid, psoralic acid-glucoside, rutin, psoralen and bergapten, respectively. The present study suggests that DESs are truly designer and efficient solvents and the method we developed was efficient and sustainable for extraction main compounds from Fig leaves.mg/g. Copyright © 2017 Elsevier B.V. All rights reserved.

Hollow Fiber Supported Liquid Membrane Extraction Combined with HPLC-UV for Simultaneous Preconcentration and Determination of Urinary Hippuric Acid and Mandelic Acid

PubMed Central

Bahrami, Abdulrahman; Ghamari, Farhad; Yamini, Yadollah; Ghorbani Shahna, Farshid; Moghimbeigi, Abbas

2017-01-01

This work describes a new extraction method with hollow-fiber liquid-phase microextraction based on facilitated pH gradient transport for analyzing hippuric acid and mandelic acid in aqueous samples. The factors affecting the metabolites extraction were optimized as follows: the volume of sample solution was 10 mL with pH 2 containing 0.5 mol·L−1 sodium chloride, liquid membrane containing 1-octanol with 20% (w/v) tributyl phosphate as the carrier, the time of extraction was 150 min, and stirring rate was 500 rpm. The organic phase immobilized in the pores of a hollow fiber was back-extracted into 24 µL of a solution containing sodium carbonate with pH 11, which was placed inside the lumen of the fiber. Under optimized conditions, the high enrichment factors of 172 and 195 folds, detection limit of 0.007 and 0.009 µg·mL−1 were obtained. The relative standard deviation (RSD) (%) values for intra- and inter-day precisions were calculated at 2.5%–8.2% and 4.1%–10.7%, respectively. The proposed method was successfully applied to the analysis of these metabolites in real urine samples. The results indicated that hollow-fiber liquid-phase microextraction (HF-LPME) based on facilitated pH gradient transport can be used as a sensitive and effective method for the determination of mandelic acid and hippuric acid in urine specimens. PMID:28208685

Comparison of whole-cell fatty acid (MIDI) or phospholipid fatty acid (PLFA) extractants as biomarkers to profile soil microbial communities.

PubMed

Fernandes, Marcelo F; Saxena, Jyotisna; Dick, Richard P

2013-07-01

The whole-cell lipid extraction to profile microbial communities on soils using fatty acid (FA) biomarkers is commonly done with the two extractants associated with the phospholipid fatty acid (PLFA) or Microbial IDentification Inc. (MIDI) methods. These extractants have very different chemistry and lipid separation procedures, but often shown a similar ability to discriminate soils from various management and vegetation systems. However, the mechanism and the chemistry of the exact suite of FAs extracted by these two methods are poorly understood. Therefore, the objective was to qualitatively and quantitatively compare the MIDI and PLFA microbial profiling methods for detecting microbial community shifts due to soil type or management. Twenty-nine soil samples were collected from a wide range of soil types across Oregon and extracted FAs by each method were analyzed by gas chromatography (GC) and GC-mass spectrometry. Unlike PLFA profiles, which were highly related to microbial FAs, the overall MIDI-FA profiles were highly related to the plant-derived FAs. Plant-associated compounds were quantitatively related to particulate organic matter (POM) and qualitatively related to the standing vegetation at sampling. These FAs were negatively correlated to respiration rate normalized to POM (RespPOM), which increased in systems under more intensive management. A strong negative correlation was found between MIDI-FA to PLFA ratios and total organic carbon (TOC). When the reagents used in MIDI procedure were tested for the limited recovery of MIDI-FAs from soil with high organic matter, the recovery of MIDI-FA microbial signatures sharply decreased with increasing ratios of soil to extractant. Hence, the MIDI method should be used with great caution for interpreting changes in FA profiles due to shifts in microbial communities.

Potential Use of Plant Waste from the Moth Orchid (Phalaenopsis Sogo Yukidian “V3”) as an Antioxidant Source

PubMed Central

Thi Tuyen, Phung; Van Quan, Nguyen; Thi Thu Ha, Pham; Thanh Quan, Nguyen; Fan, Xinyan; Mai Van, Truong; Dang Khanh, Tran

2017-01-01

This research was conducted to exploit the waste of used plant parts from the widely marketed moth orchid cultivar (Phalaenopsis Sogo Yukidian “V3”). Various extracts of roots, stems, and leaves were evaluated for total phenolics, total flavonoids, and antioxidant capacity. The bound extract from stems contained the highest total phenolics (5.092 ± 0.739 mg GAE (gallic acid equivalent)/g DW (dry weight)). The maximum total flavonoids (2.218 ± 0.021 mg RE (rutin equivalent)/g DW) were found in the hexane extract of leaves. Ethyl acetate extract from roots showed the greatest antioxidant activity compared to other extracts. Of these extracts, the IC50 values of these samples were 0.070 mg/mL, and 0.450 mg/mL in a free radical 1,-diphenyl-picryl-hydrazyl (DPPH) assay and reducing power method, respectively. The lipid peroxidation inhibition (LPI) was found to be 94.2% using the β-carotene bleaching method. Five phenolic compounds including caffeic acid, syringic acid, vanillin, ellagic acid, and cinnamic acid were quantified by high performance liquid chromatography (HPLC). It is suggested that the roots of the hybrid Phalaenopsis Sogo Yukidian “V3” cultivar may be exploited as an effective source of antioxidants. PMID:28953245

Molecularly imprinted polymers with synthetic dummy template for simultaneously selective removal and enrichment of ginkgolic acids from Ginkgo biloba L. leaves extracts.

PubMed

Ji, Wenhua; Ma, Xiuli; Xie, Hongkai; Chen, Lingxiao; Wang, Xiao; Zhao, Hengqiang; Huang, Luqi

2014-11-14

Dummy molecularly imprinted polymers (DMIPs) for simultaneously selective removal and enrichment of ginkgolic acids (GAs) during the processing of Ginkgo biloba leaves have been prepared. Two dummy template molecule with similar structural skeleton to GAs, 6-methoxysalicylic acid (MOSA, DT-1) and 6-hexadecyloxysalicylic acid (HOSA, DT-2), have been designed and synthesized. The performance of the DMIPs and NIPs were evaluated including selective recognition capacity, adsorption isotherm, and adsorption kinetics. The selective recognition capacity of the three GAs with four analogues on the sorbents illustrated that the DMIPs sorbents have high specificity for GAs. An efficient method based on DMIP-HOSA coupled with solid-phase extraction (SPE) was developed for simultaneously selective removal and enrichment of ginkgolic acids (GAs) during the processing of Ginkgo biloba leaves. The method showed excellent recoveries (82.5-88.7%) and precision (RSD 0.5-2.6%, n=5) for licorice extracts, Gastrodia elata extracts and pepper extracts spiked at three concentration levels each (50, 100, 200 μg mL(-1)). The results indicated that GAs and standardized Ginkgo biloba leaves extracts could be obtained simultaneously through the DMIP-SPE. Copyright © 2014 Elsevier B.V. All rights reserved.

HPLC-PDA analysis and anti-inflammatory effects of Mori Cortex Radicis.

PubMed

Seo, Chang-Seob; Lim, Hye-Sun; Jeong, Soo-Jin; Ha, Hyekyung; Shin, Hyeun-Kyoo

2013-10-01

Mori Cortex Radicis (MCR, Moraceae) is used traditionally in the treatment ofjaundice, hematemesis, edema, and pollakisuria in Korea. In this study, the antiinflammatory effects of MCR extract were investigated using RAW 264.7 cells. The simultaneous analysis of five components present (neochlorogenic acid, chlorogenic acid, cryptochlorogenic acid, caffeic acid, and p-coumaric acid) in the MCR extract was performed using high-performance liquid chromatography (HPLC) coupled with photodiode array (PDA) detection. We determined the effects of MCR extract and its components on the production of nitric oxide (NO), prostaglandin E2 (PGE2), and mRNA expression of cyclooxygenase-2 (COX-2) in RAW 264.7 cells. MCR extract suppressed the production of NO and PGE2 in RAW 264.7 cells in a dose-dependent manner. None of the five components of the MCR extract had any influence on the production of NO. However, caffeic acid and p-coumaric acid inhibited the production of PGE2 and mRNA expression of COX-2 in RAW 264.7 cells. Our results suggest that MCR extract may offer potential as a therapeutic agent for the treatment of inflammation. The method we have established will help to improve the quality control of MCR extracts.

An assessment of the liquid-gas partitioning behavior of major wastewater odorants using two comparative experimental approaches: liquid sample-based vaporization vs. impinger-based dynamic headspace extraction into sorbent tubes.

PubMed

Iqbal, Mohammad Asif; Kim, Ki-Hyun; Szulejko, Jan E; Cho, Jinwoo

2014-01-01

The gas-liquid partitioning behavior of major odorants (acetic acid, propionic acid, isobutyric acid, n-butyric acid, i-valeric acid, n-valeric acid, hexanoic acid, phenol, p-cresol, indole, skatole, and toluene (as a reference)) commonly found in microbially digested wastewaters was investigated by two experimental approaches. Firstly, a simple vaporization method was applied to measure the target odorants dissolved in liquid samples with the aid of sorbent tube/thermal desorption/gas chromatography/mass spectrometry. As an alternative method, an impinger-based dynamic headspace sampling method was also explored to measure the partitioning of target odorants between the gas and liquid phases with the same detection system. The relative extraction efficiency (in percent) of the odorants by dynamic headspace sampling was estimated against the calibration results derived by the vaporization method. Finally, the concentrations of the major odorants in real digested wastewater samples were also analyzed using both analytical approaches. Through a parallel application of the two experimental methods, we intended to develop an experimental approach to be able to assess the liquid-to-gas phase partitioning behavior of major odorants in a complex wastewater system. The relative sensitivity of the two methods expressed in terms of response factor ratios (RFvap/RFimp) of liquid standard calibration between vaporization and impinger-based calibrations varied widely from 981 (skatole) to 6,022 (acetic acid). Comparison of this relative sensitivity thus highlights the rather low extraction efficiency of the highly soluble and more acidic odorants from wastewater samples in dynamic headspace sampling.

Current lipid extraction methods are significantly enhanced adding a water treatment step in Chlorella protothecoides.

PubMed

Ren, Xiaojie; Zhao, Xinhe; Turcotte, François; Deschênes, Jean-Sébastien; Tremblay, Réjean; Jolicoeur, Mario

2017-02-11

Microalgae have the potential to rapidly accumulate lipids of high interest for the food, cosmetics, pharmaceutical and energy (e.g. biodiesel) industries. However, current lipid extraction methods show efficiency limitation and until now, extraction protocols have not been fully optimized for specific lipid compounds. The present study thus presents a novel lipid extraction method, consisting in the addition of a water treatment of biomass between the two-stage solvent extraction steps of current extraction methods. The resulting modified method not only enhances lipid extraction efficiency, but also yields a higher triacylglycerols (TAG) ratio, which is highly desirable for biodiesel production. Modification of four existing methods using acetone, chloroform/methanol (Chl/Met), chloroform/methanol/H 2 O (Chl/Met/H 2 O) and dichloromethane/methanol (Dic/Met) showed respective lipid extraction yield enhancement of 72.3, 35.8, 60.3 and 60.9%. The modified acetone method resulted in the highest extraction yield, with 68.9 ± 0.2% DW total lipids. Extraction of TAG was particularly improved with the water treatment, especially for the Chl/Met/H 2 O and Dic/Met methods. The acetone method with the water treatment led to the highest extraction level of TAG with 73.7 ± 7.3 µg/mg DW, which is 130.8 ± 10.6% higher than the maximum value obtained for the four classical methods (31.9 ± 4.6 µg/mg DW). Interestingly, the water treatment preferentially improved the extraction of intracellular fractions, i.e. TAG, sterols, and free fatty acids, compared to the lipid fractions of the cell membranes, which are constituted of phospholipids (PL), acetone mobile polar lipids and hydrocarbons. Finally, from the 32 fatty acids analyzed for both neutral lipids (NL) and polar lipids (PL) fractions, it is clear that the water treatment greatly improves NL-to-PL ratio for the four standard methods assessed. Water treatment of biomass after the first solvent extraction step helps the subsequent release of intracellular lipids in the second extraction step, thus improving the global lipids extraction yield. In addition, the water treatment positively modifies the intracellular lipid class ratios of the final extract, in which TAG ratio is significantly increased without changes in the fatty acids composition. The novel method thus provides an efficient way to improve lipid extraction yield of existing methods, as well as selectively favoring TAG, a lipid of the upmost interest for biodiesel production.

Extracting metals directly from metal oxides

DOEpatents

Wai, Chien M.; Smart, Neil G.; Phelps, Cindy

1997-01-01

A method of extracting metals directly from metal oxides by exposing the oxide to a supercritical fluid solvent containing a chelating agent is described. Preferably, the metal is an actinide or a lanthanide. More preferably, the metal is uranium, thorium or plutonium. The chelating agent forms chelates that are soluble in the supercritical fluid, thereby allowing direct removal of the metal from the metal oxide. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is selected from the group consisting of .beta.-diketones, halogenated .beta.-diketones, phosphinic acids, halogenated phosphinic acids, carboxylic acids, halogenated carboxylic acids, and mixtures thereof. In especially preferred embodiments, at least one of the chelating agents is fluorinated. The method provides an environmentally benign process for removing metals from metal oxides without using acids or biologically harmful solvents. The chelate and supercritical fluid can be regenerated, and the metal recovered, to provide an economic, efficient process.

Extracting metals directly from metal oxides

DOEpatents

Wai, C.M.; Smart, N.G.; Phelps, C.

1997-02-25

A method of extracting metals directly from metal oxides by exposing the oxide to a supercritical fluid solvent containing a chelating agent is described. Preferably, the metal is an actinide or a lanthanide. More preferably, the metal is uranium, thorium or plutonium. The chelating agent forms chelates that are soluble in the supercritical fluid, thereby allowing direct removal of the metal from the metal oxide. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent is selected from the group consisting of {beta}-diketones, halogenated {beta}-diketones, phosphinic acids, halogenated phosphinic acids, carboxylic acids, halogenated carboxylic acids, and mixtures thereof. In especially preferred embodiments, at least one of the chelating agents is fluorinated. The method provides an environmentally benign process for removing metals from metal oxides without using acids or biologically harmful solvents. The chelate and supercritical fluid can be regenerated, and the metal recovered, to provide an economic, efficient process. 4 figs.

Highly efficient extraction of anthocyanins from grape skin using deep eutectic solvents as green and tunable media.

PubMed

Jeong, Kyung Min; Zhao, Jing; Jin, Yan; Heo, Seong Rok; Han, Se Young; Yoo, Da Eun; Lee, Jeongmi

2015-12-01

Deep eutectic solvents (DESs) were investigated as tunable, environmentally benign, yet superior extraction media to enhance the extraction of anthocyanins from grape skin, which is usually discarded as waste. Ten DESs containing choline chloride as hydrogen bond acceptor combined with different hydrogen bond donors were screened for high extraction efficiencies based on the anthocyanin extraction yields. As a result, citric acid, D-(+)-maltose, and fructose were selected as the effective DES components, and the newly designed DES, CM-6 that is composed of citric acid and D-(+)-maltose at 4:1 molar ratio, exhibited significantly higher levels of anthocyanin extraction yields than conventional extraction solvents such as 80% aqueous methanol. The final extraction method was established based on the ultrasound-assisted extraction under conditions optimized using response surface methodology. Its extraction yields were double or even higher than those of conventional methods that are time-consuming and use volatile organic solvents. Our method is truly a green method for anthocyanin extraction with great extraction efficiency using a minimal amount of time and solvent. Moreover, this study suggested that grape skin, the by-products of grape juice processing, could serve as a valuable source for safe, natural colorants or antioxidants by use of the eco-friendly extraction solvent, CM-6.

In vitro and in vivo evaluation of the antioxidant and prooxidant activity of phenolic compounds obtained from grape (Vitis vinifera) pomace.

PubMed

Cotoras, Milena; Vivanco, Herman; Melo, Ricardo; Aguirre, María; Silva, Evelyn; Mendoza, Leonora

2014-12-16

The antioxidant and/or prooxidant ability of extracts obtained from wine waste were analyzed using in vitro and in vivo assays. Cyclic voltammetry was used as the in vitro assay to determine the antioxidant and/or prooxidant properties and, the in vivo effect on mycelial growth of the fungus Botrytis cinerea was evaluated. In addition, the prooxidant activity was evaluated by intracellular oxidation of compound 2,7-dichlorodihydrofluorescein diacetate (DCFH-DA) in B. cinerea. The extracts used in this study were obtained from grape pomace of Cabernet Sauvignon, Carménère and Syrah varieties from the Misiones de Rengo Vineyard by simple extraction, using methanol/HCl 1% (v/v), ethanol 70% (v/v), or Soxhlet extraction. According to the results obtained, gallic acid was the most represented phenolic compound independent of grape variety and extraction method. In addition, vanillic acid; protocatechuic acid, syringic acid, quercetin and kaempferol were found in the extracts. From this study it was possible concluded that, depending of the method of extraction of the grape residues and the grape variety (Cabernet Sauvignon, Carménère and Syrah), the extracts showed antioxidant and/or prooxidant activity. However, no correlation can be established between the anodic oxidation potentials of the extracts and their effect on the fungus B. cinerea.

Solvent Extraction of Furfural From Biomass

NASA Technical Reports Server (NTRS)

Humphrey, M. F.

1984-01-01

Solvent-extraction method reduces energy required to remove furfural produced during acid hydrolysis of biomass. Acid hydrolysis performed in vessel containing both solvents and reacting ingredients. With intimate contact between solvents and aqueous hydrolyis liqour, furfural removed form liquor almost as fast as it forms.

Freeze-out extraction of monocarboxylic acids from water into acetonitrile under the action of centrifugal forces

NASA Astrophysics Data System (ADS)

Bekhterev, V. N.

2016-10-01

It is established that the efficiency of the freezing-out extraction of monocarboxylic acids C3-C;8 and sorbic acid from water into acetonitrile increases under the action of centrifugal forces. The linear growth of the partition coefficient in the homologous series of C2-C8 acids with an increase in molecule length, and the difference between the efficiency of extracting sorbic and hexanoic acid, are discussed using a theoretical model proposed earlier and based on the adsorption-desorption equilibrium of the partition of dissolved organic compounds between the resulting surface of ice and the liquid phase of the extract. The advantages of the proposed technique with respect to the degree of concentration over the method of low-temperature liquid-liquid extraction are explained in light of the phase diagram for the water-acetonitrile mixture.

Preparation of Formalin-fixed Paraffin-embedded Tissue Cores for both RNA and DNA Extraction.

PubMed

Patel, Palak G; Selvarajah, Shamini; Boursalie, Suzanne; How, Nathan E; Ejdelman, Joshua; Guerard, Karl-Philippe; Bartlett, John M; Lapointe, Jacques; Park, Paul C; Okello, John B A; Berman, David M

2016-08-21

Formalin-fixed paraffin embedded tissue (FFPET) represents a valuable, well-annotated substrate for molecular investigations. The utility of FFPET in molecular analysis is complicated both by heterogeneous tissue composition and low yields when extracting nucleic acids. A literature search revealed a paucity of protocols addressing these issues, and none that showed a validated method for simultaneous extraction of RNA and DNA from regions of interest in FFPET. This method addresses both issues. Tissue specificity was achieved by mapping cancer areas of interest on microscope slides and transferring annotations onto FFPET blocks. Tissue cores were harvested from areas of interest using 0.6 mm microarray punches. Nucleic acid extraction was performed using a commercial FFPET extraction system, with modifications to homogenization, deparaffinization, and Proteinase K digestion steps to improve tissue digestion and increase nucleic acid yields. The modified protocol yields sufficient quantity and quality of nucleic acids for use in a number of downstream analyses, including a multi-analyte gene expression platform, as well as reverse transcriptase coupled real time PCR analysis of mRNA expression, and methylation-specific PCR (MSP) analysis of DNA methylation.

Alkaline earth cation extraction from acid solution

DOEpatents

Dietz, Mark; Horwitz, E. Philip

2003-01-01

An extractant medium for extracting alkaline earth cations from an aqueous acidic sample solution is described as are a method and apparatus for using the same. The separation medium is free of diluent, free-flowing and particulate, and comprises a Crown ether that is a 4,4'(5')[C.sub.4 -C.sub.8 -alkylcyclohexano]18-Crown-6 dispersed on an inert substrate material.

Rosmarinic acid content in antidiabetic aqueous extract of Ocimum canum sims grown in Ghana.

PubMed

Berhow, Mark A; Affum, Andrews Obeng; Gyan, Ben A

2012-07-01

Rosmarinic acid (RA) is an important antioxidant polyphenol that is found in a variety of spices and herbs, including Ocimum canum Sims (locally called eme or akokobesa in Ghana). Aqueous extracts from the leaves of O. canum are used as an antidiabetic herbal medicine in Ghana. Analytical thin-layer chromatography was used to examine the composition of the polyphenols in leaf extracts. The polyphenol content in the aqueous and methanol extracts from the leaf, as determined by the Folin-Ciocalteu method, were 314 and 315 mg gallic acid equivalent/g leaf sample, respectively. The total flavonoid concentration as determined by the aluminum(III) chloride method was 135 mg catechin equivalent/g leaf sample. High-performance liquid chromatography coupled to an electrospray Quadrupole time-of-flight mass spectrometer was also used to determine the polyphenol fingerprint profile in the leaf extracts of O. canum. Although the average RA concentration in the O. canum leaf extracts from Ghana was 1.69 mg/g dry weight (reported values range from 0.01 to 99.62 mg/g dry weight), this polyphenol was still a prominent peak in addition to caffeic acid derivatives.

Extraction of pectin from passion fruit rind (Passiflora edulis var. flavicarpa Degener) for edible coating

NASA Astrophysics Data System (ADS)

Inayati, Puspita, Rifka Intan; Fajrin, Vika Latifiana

2018-02-01

One of fruit preservation method is by applying the edible coating. Rind of passion fruit (Passiflora edulis var. flavicarpa Degener), which is kind of waste, can be utilized as edible coating through pectin extraction process. The purposes of this work were to determine the suitable solvent for the pectin extraction and techniques for applying the produced edible coating on strawberry, to produce edible coating from the pectin, and the test the performance of the edible coating which was applied to strawberries. Pectin from passion fruit rind was collected through conventional extraction method using two types of solvent, i.e. acetic acid solution and hydrochloric acid solution with concentration of 0.01 N, 0.015 N, 0.02 N, 0.025 N, and 0.03 N. The results showed that chloric acid solution was more suitable for the pectin extraction from passion fruit. Maximum yield of 30.78% was obtained at hydrochloric acid concentration of 0.02 N. Obtained pectin from the extraction was then processed into the edible coating by adding plasticizers and calcium chloride dihydrate. Storability of the coated strawberry was observed to measure the performance of the edible coating

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction

PubMed Central

Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

2017-01-01

The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%–61.85%) and oleic acid (1.64%–18.97%). Thymoquinone (0.72%–21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly (P<0.05) higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique. PMID:28814830

Comparative analysis of essential oil composition of Iranian and Indian Nigella sativa L. extracted using supercritical fluid extraction and solvent extraction.

PubMed

Ghahramanloo, Kourosh Hasanzadeh; Kamalidehghan, Behnam; Akbari Javar, Hamid; Teguh Widodo, Riyanto; Majidzadeh, Keivan; Noordin, Mohamed Ibrahim

2017-01-01

The objective of this study was to compare the oil extraction yield and essential oil composition of Indian and Iranian Nigella sativa L. extracted by using Supercritical Fluid Extraction (SFE) and solvent extraction methods. In this study, a gas chromatography equipped with a mass spectrophotometer detector was employed for qualitative analysis of the essential oil composition of Indian and Iranian N. sativa L. The results indicated that the main fatty acid composition identified in the essential oils extracted by using SFE and solvent extraction were linoleic acid (22.4%-61.85%) and oleic acid (1.64%-18.97%). Thymoquinone (0.72%-21.03%) was found to be the major volatile compound in the extracted N. sativa oil. It was observed that the oil extraction efficiency obtained from SFE was significantly ( P <0.05) higher than that achieved by the solvent extraction technique. The present study showed that SFE can be used as a more efficient technique for extraction of N. Sativa L. essential oil, which is composed of higher linoleic acid and thymoquinone contents compared to the essential oil obtained by the solvent extraction technique.

α-Glucosidase enzyme inhibitory effects and ursolic and oleanolic acid contents of fourteen Anatolian Salvia species.

PubMed

Kalaycıoğlu, Zeynep; Uzaşçı, Sesil; Dirmenci, Tuncay; Erim, F Bedia

2018-06-05

During the last decade, ursolic and oleanolic acids have been of considerable interest because of their α-glucosidase inhibitory activities and potential effects for treatment of type 2 diabetes. A simple and sensitive reversed-phase HPLC method was developed for the simultaneous determination of ursolic acid and oleanolic acid. The optimal mobile phase was selected as 85% acetonitrile solution. The limit of detection of the method for ursolic acid and oleanolic acid were 14 ng mL -1 and 13 ng mL -1 , respectively. The method showed good precision and accuracy with intra-day and inter-day variations of 0.54% and 7.33% for ursolic acid, intra-day and inter-day variations of 0.51% and 5.26% for oleanolic acid, and overall recoveries of 97.8% and 98.5% for ursolic acid and oleanolic acid, respectively. Application of the method to determine the ursolic acid and oleanolic acid contents in the Salvia species revealed both compounds, with varying amounts between 0.21-9.76 mg g -1 ursolic acid and 0.20-12.7 mg g -1 oleanolic acid, respectively, among 14 Salvia species analyzed. Additionally, the plant extracts were analyzed for their inhibitory activities on α-glucosidase. According to the results of this assay, the extracts showed considerable activity on α-glucosidase with IC 50 values from 17.6 to 173 μg mL -1 . A strong negative correlation was detected between the amounts of both acids and IC 50 values of extracts. Anatolian Salvia species have great potential as functional plants in the management of diabetes. Copyright © 2018 Elsevier B.V. All rights reserved.

Selectively Adsorptive Extraction of Phenylarsonic Acids in Chicken Tissue by Carboxymethyl α-Cyclodextrin Immobilized Fe3O4 Magnetic Nanoparticles Followed Ultra Performance Liquid Chromatography Coupled Tandem Mass Spectrometry Detection

PubMed Central

Jia, Jing; Zhang, Wei; Wang, Jing; Wang, Peilong; Zhu, Ruohua

2014-01-01

Carboxymethyl α-cyclodextrin immobilized Fe3O4 magnetic nanoparticles (CM-α-CD-Fe3O4) were synthesized for the selectively adsorptive extraction of five phenylarsonic acids including p-amino phenylarsonic acid, p-nitro phenylarsonic acid, p-hydroxy phenylarsonic acid, p-acylamino phenylarsonic acid and p-hydroxy-3-nitro phenylarsonic acid in chicken tissue. Using ultra performance liquid chromatography coupled with tandem mass spectrometry (UPLC-MS/MS), a highly sensitive analytical method was proposed for the determination of five phenylarsonic acids. It was shown that CM-α-CD-Fe3O4 could extract the five phenylarsonic acids in complex chicken tissue samples with high extraction efficiency. Under the optimal conditions, a high enrichment factor, ranging from 349 to 606 fold, was obtained. The limits of detection (LODs) (at a signal-to-noise ratio of 3) were in the range of 0.05–0.11 µg/kg for the five phenylarsonic acids. The proposed method was applied for the determination of five target phenylarsonic acids in chicken muscle and liver samples. Recoveries for the spiked samples with 0.2 µg/kg, 2.0 µg/kg and 20 µg/kg of each phenylarsonic acids were in the range of 77.2%–110.2%, with a relative standard deviation (RSD) of less than 12.5%. PMID:25215503

Detection of Salmonella spp. and Listeria monocytogenes in Suspended Organic Waste by Nucleic Acid Extraction and PCR

PubMed Central

Burtscher, Carola; Fall, Papa A.; Wilderer, Peter A.; Wuertz, Stefan

1999-01-01

A nucleic acid-based method for the detection of the bacterial pathogens Salmonella spp. and Listeria monocytogenes in biological waste was developed. The detection limits were less than 10 cells per ml of biological waste. The method does not include a phenol extraction step and can be easily performed in 1 to 2 days. PMID:10224026

Development of a simple and valid method for the trace determination of phthalate esters in human plasma using dispersive liquid-liquid microextraction coupled with gas chromatography-mass spectrometry.

PubMed

Ebrahim, Karim; Poursafa, Parinaz; Amin, Mohammad Mehdi

2017-11-01

A new method was developed for the trace determination of phthalic acid esters in plasma using dispersive liquid-liquid microextraction and gas chromatography with mass spectrometry analysis. Plasma proteins were efficiently precipitated by trichloroacetic acid and then a mixture of chlorobenzene (as extraction solvent) and acetonitrile (as dispersive solvent) rapidly injected to clear supernatant using a syringe. After centrifuging, chlorobenzene sedimented at the bottom of the test tube. 1 μL of this sedimented phase was injected into the gas chromatograph for phthalic acid esters analysis. Different factors affecting the extraction performance, such as the type of extraction and dispersive solvent, their volume, extraction time, and the effects of salt addition were investigated and optimized. Under the optimum conditions, the enrichment factors and extraction recoveries were satisfactory and ranged between 820-1020 and 91-97%, respectively. The linear range was wide (50-1000 ng/mL) and limit of detection was very low (1.5-2.5 ng/mL for all analytes). The relative standard deviations for analysis of 1 μg/mL of the analytes were between 3.2-6.1%. Salt addition showed no significant effect on extraction recovery. Finally, the proposed method was successfully utilized for the extraction and determination of the phthalic acid esters in human plasma samples and satisfactory results were obtained. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

HPLC method for the simultaneous quantification of the major organic acids in Angeleno plum fruit

NASA Astrophysics Data System (ADS)

Wang, Yanwei; Wang, Jing; Cheng, Wei; Zhao, Zhilei; Cao, Jiankang

2014-08-01

A method was developed to profile major organic acids in Angeleno fruit by high performance liquid chromatography. Organic acids in plum were extracted by water with ultra- sonication at 50°C for 30 min. The extracts were chromatographed on Waters Atlantis T3 C18 column (4.6 mm×250 mm, 5 μm) with 0.01mol/L sulfuric acid and water as mobile phase, and flow rate was 0.5 ml/min. The column temperature was 40C, and chromatography was monitored by a diode array detector at 210 nm. The result showed that malic acid, citric acid, tartaric acid, oxalic acid, pyruvic acid, acetic acid, succinic acid in Angeleno plum, and the malic acid was the major organic acids. The coefficient of determination of the standard calibration curve is R2 > 0.999. The organic acids recovery ranged from 99.11% for Malic acid to 106.70% for Oxalic acid, and CV (n=6) ranged from 0.95% for Malic acid to 6.23% for Oxalic acid, respectively. The method was accurate, sensitive and feasible in analyzing the organic acids in Angeleno plum.

Statistical evaluation of fatty acid profile and cholesterol content in fish (common carp) lipids obtained by different sample preparation procedures.

PubMed

Spiric, Aurelija; Trbovic, Dejana; Vranic, Danijela; Djinovic, Jasna; Petronijevic, Radivoj; Matekalo-Sverak, Vesna

2010-07-05

Studies performed on lipid extraction from animal and fish tissues do not provide information on its influence on fatty acid composition of the extracted lipids as well as on cholesterol content. Data presented in this paper indicate the impact of extraction procedures on fatty acid profile of fish lipids extracted by the modified Soxhlet and ASE (accelerated solvent extraction) procedure. Cholesterol was also determined by direct saponification method, too. Student's paired t-test used for comparison of the total fat content in carp fish population obtained by two extraction methods shows that differences between values of the total fat content determined by ASE and modified Soxhlet method are not statistically significant. Values obtained by three different methods (direct saponification, ASE and modified Soxhlet method), used for determination of cholesterol content in carp, were compared by one-way analysis of variance (ANOVA). The obtained results show that modified Soxhlet method gives results which differ significantly from the results obtained by direct saponification and ASE method. However the results obtained by direct saponification and ASE method do not differ significantly from each other. The highest quantities for cholesterol (37.65 to 65.44 mg/100 g) in the analyzed fish muscle were obtained by applying direct saponification method, as less destructive one, followed by ASE (34.16 to 52.60 mg/100 g) and modified Soxhlet extraction method (10.73 to 30.83 mg/100 g). Modified Soxhlet method for extraction of fish lipids gives higher values for n-6 fatty acids than ASE method (t(paired)=3.22 t(c)=2.36), while there is no statistically significant difference in the n-3 content levels between the methods (t(paired)=1.31). The UNSFA/SFA ratio obtained by using modified Soxhlet method is also higher than the ratio obtained using ASE method (t(paired)=4.88 t(c)=2.36). Results of Principal Component Analysis (PCA) showed that the highest positive impact to the second principal component (PC2) is recorded by C18:3 n-3, and C20:3 n-6, being present in a higher amount in the samples treated by the modified Soxhlet extraction, while C22:5 n-3, C20:3 n-3, C22:1 and C20:4, C16 and C18 negatively influence the score values of the PC2, showing significantly increased level in the samples treated by ASE method. Hotelling's paired T-square test used on the first three principal components for confirmation of differences in individual fatty acid content obtained by ASE and Soxhlet method in carp muscle showed statistically significant difference between these two data sets (T(2)=161.308, p<0.001). Copyright 2010 Elsevier B.V. All rights reserved.

Pressurized liquid extraction and chemical characterization of safflower oil: A comparison between methods.

PubMed

Conte, Rogério; Gullich, Letícia M D; Bilibio, Denise; Zanella, Odivan; Bender, João P; Carniel, Naira; Priamo, Wagner L

2016-12-15

This work investigates the extraction process of safflower oil using pressurized ethanol, and compares the chemical composition obtained (in terms of fatty acids) with other extraction techniques. Soxhlet and Ultrasound showed maximum global yield of 36.53% and 30.41%, respectively (70°C and 240min). PLE presented maximum global yields of 25.62% (3mLmin(-1)), 19.94% (2mLmin(-1)) and 12.37% (1mLmin(-1)) at 40°C, 100bar and 60min. Palmitic acid showed the lower concentration in all experimental conditions (from 5.70% to 7.17%); Stearic and Linoleic acid presented intermediate concentrations (from 2.93% to 25.09% and 14.09% to 19.06%, respectively); Oleic acid showed higher composition (from 55.12% to 83.26%). Differences between percentages of fatty acids, depending on method were observed. Results may be applied to maximize global yields and select fatty acids, reducing the energetic costs and process time. Copyright © 2016 Elsevier Ltd. All rights reserved.

Hawthorn ethanolic extracts with triterpenoids and flavonoids exert hepatoprotective effects and suppress the hypercholesterolemia-induced oxidative stress in rats

PubMed Central

Rezaei-Golmisheh, Ali; Malekinejad, Hassan; Asri-Rezaei, Siamak; Farshid, Amir Abbas; Akbari, Peyman

2015-01-01

Objective(s): The current study was aimed to determine the bioactive constituents and biological effects of the Crataegus monogyna ethanolic extracts from bark, leaves and berries on hypercholesterolemia. Materials and Methods: Oleanolic acid, ursolic acid, quercetin and lupeol concentrations were quantified by HPLC. Total phenol content and radical scavenging activity of extracts were also measured. The hypocholesterolemic, antioxidant, and hepatoprotective effects of the extracts were examined in hypercholesterolemic rats and compared with orlistat. Results: The highest phenol content, oleanolic acid, quercetin and lupeol levels and free radical scavenging potency were found in the bark extract, and the highest ursolic acid level was found in the berries extract. Orlistat and extracts significantly (P<0.05) lowered the hypercholesterolemia-increased serum level of hepatic enzymes and lipid peroxidation level. Hawthorn’s extracts protected from hepatic thiol depletion and improved the lipid profile and hepatic damages. Conclusion: Data suggested that hawthorn’s extracts are able to protect from hypercholesterolemia-induced oxidative stress and hepatic injuries. Moreover, the hypocholesterolemic effect of extracts was found comparable to orlistat. PMID:26361538

Antitumor activity of Annona squamosa seed oil.

PubMed

Chen, Yong; Chen, Yayun; Shi, Yeye; Ma, Chengyao; Wang, Xunan; Li, Yue; Miao, Yunjie; Chen, Jianwei; Li, Xiang

2016-12-04

Custard apple (Annona squamosa Linn.) is an edible tropical fruit, and its seeds have been used to treat "malignant sore" (cancer) and other usage as insecticide. A comparison of extraction processes, chemical composition analysis and antitumor activity of A. squamosa seed oil (ASO) were investigated. The optimal extraction parameters of ASO were established by comparing percolation, soxhlet, ultrasonic and SFE-CO 2 extraction methods. The chemical composition of fatty acid and content of total annonaceous acetogenins (ACGs) of ASO was investigated by GC-MS and colorimetric assay, and anti-tumor activity of ASO was tested using H 22 xenografts bearing mice. The optimal extraction parameters of ASO were obtained as follows: using soxhlet extraction method with extraction solvent of petroleum ether, temperature of 80°C, and extraction time of 90min. Under these conditions, the yield of ASO was 22.65%. GC-MS analysis results showed that the main chemical compositions of fatty acid of ASO were palmitic acid (9.92%), linoleic acid (20.49%), oleic acid (56.50%) and stearic acid (9.14%). The total ACGs content in ASO was 41.00mg/g. ASO inhibited the growth of H 22 tumor cells in mice with a maximum inhibitory rate of 53.54% by oral administration. Furthermore, it was found that ASO exerted an antitumor effect via decreasing interleukin-6 (IL-6), janus kinase (Jak) and phosphorylated signal transducers and activators of transcription (p-Stat3) expression. The results demonstrated that ASO suppressed the H 22 solid tumor development may due to its main chemical constituents unsaturated fatty acid and ACGs via IL-6/Jak/Stat3 pathway. ASO may be a potential candidate for the treatment of cancer. Copyright © 2016 Elsevier Ireland Ltd. All rights reserved.

Antioxidant potential of mulberry and non-mulberry silk sericin and its implications in biomedicine.

PubMed

Kumar, Jadi Praveen; Mandal, Biman B

2017-07-01

Sericin, a principal constituent of silk, is widely used in various biomedical applications. In addition, conferring protection against free radicals and oxidative damage add more value to its therapeutic potential. However, the antioxidant (AO) properties of silk sericin (SS) remains contingent on extraction procedures. In the present study, we have evaluated the effect of different extraction methods (conventional, autoclaving, urea, alkali and acid-degradation) on AO properties of SS from three Indian silk varieties [Antheraea assamensis (AA), Philosamia ricini (PR) and Bombyx mori (BM)]. The physico-chemical characterization studies revealed that the molecular weight of SS isolates of each method ranged from 10 to 220kDa along with varied protein structural biochemistry. SS extracts using urea-degradation (BM, PR and AA), conventional method and alkali-degradation (BM) displayed high percentage of β-sheets, random coils and turns. Acid-degraded SS (PR, followed by AA and BM) showed the highest total flavonoid content while conventional method (PR), autoclaving (AA) and alkali-degradation (BM) displayed lowest flavonoid levels. Interestingly, SS extracted by autoclaving (BM and AA), acid-degradation (PR), conventional and alkali-degradation (BM, AA and PR) methods exhibited 50% reduction of 2, 2-diphenyl-1-picrylhydrazyl (DPPH) radical. Moreover, the efficacy of antioxidant potential of SS extracted by different methods was found to be in the order of "alkali>autoclaving>conventional" as demonstrated in L929 cells. Correspondingly, the anti-lipid peroxidation activity of SS extracted by alkali method (AA, BM and PR) further confirmed better AO properties amid others. Thus, the present study demonstrates that the extraction methods may significantly affect AO activity of SS which might be of importance for potential cosmetic applications. Copyright © 2017 Elsevier Inc. All rights reserved.

Determination of silver in soils, sediments, and rocks by organic-chelate extraction and atomic absorption spectrophotometry

USGS Publications Warehouse

Chao, T.T.; Ball, J.W.; Nakagawa, H.M.

1971-01-01

A useful method for the determination of silver in soil, sediment, and rock samples in geochemical exploration has been developed. The sample is digested with concentrated nitric acid, and the silver extracted with triisooctyl thiophosphate (TOTP) in methyl isobutyl ketone (MIBK) after dilution of the acid digest to approximately 6 M. The extraction of silver into the organic extractant is quantitative and not affected by the nitric acid concentration from 4 M to 8 M, or by different volumes of TOTP-MIBK. The extracted silver is stable and remains in the organic phase up to several days. The silver concentration is determined by atomic absorption spectrophotometry. ?? 1971.

Phenylboronic acid modified solid-phase extraction column: Preparation, characterization, and application to the analysis of amino acids in sepia capsule by removing the maltose.

PubMed

Guo, Mengzhe; Yin, Dengyang; Han, Jie; Zhang, Liyan; Li, Xiao; He, Dandan; Du, Yan; Tang, Daoquan

2016-09-01

Maltose, a common auxiliary material of pharmaceutical preparation, may disturb the analysis of total amino acids in sepia capsule by aldolization. Therefore, it is necessary to remove the maltose through a convenient method. In this work, a phenylboronic acid modified solid-phase extraction column has been synthesized and used to remove the maltose. The materials were synthesized by one step "thiol-ene" reaction and the parameters of the column such as absorption capacity, recovery, and absorption specificity have been investigated. The results showed the column (0.5 cm of length × 0.5 cm of inner diameter) can absorb 4.6 mg maltose with a linear absorption and absorption specificity. Then this technique was applied in the quantification of amino acids in sepia capsule. After the optimization of the method, four kinds of amino acids, which were the most abundant, were quantified by high-performance liquid chromatography with diode array detection. The amounts of the four kinds of amino acids are 1.5∼2 times more than that without the treatment of solid-phase extraction column, which almost overcomes the influence of the maltose. All the results indicate that the phenylboronic acid modified solid-phase extraction column can successfully help to accurately quantify the total amino acids in sepia capsule. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Capillary electrophoresis method for the analysis of organic acids and amino acids in the presence of strongly alternating concentrations of aqueous lactic acid.

PubMed

Laube, Hendrik; Boden, Jana; Schneider, Roland

2017-07-01

During the production of bio-based bulk chemicals, such as lactic acid (LA), organic impurities have to be removed to produce a ready-to-market product. A capillary electrophoresis method for the simultaneous detection of LA and organic impurities in less than 10 min was developed. LA and organic impurities were detected using a direct UV detection method with micellar background electrolyte, which consisted of borate and sodium dodecyl sulfate. We investigated the effects of electrolyte composition and temperature on the speed, sensitivity, and robustness of the separation. A few validation parameters, such as linearity, limit of detection, and internal and external standards, were evaluated under optimized conditions. The method was applied for the detection of LA and organic impurities, including tyrosine, phenylalanine, and pyroglutamic acid, in samples from a continuous LA fermentation process from post-extraction tapioca starch and yeast extract.

Phenolic and triterpenoid antioxidants from Origanum majorana L. herb and extracts obtained with different solvents.

PubMed

Vági, E; Rapavi, E; Hadolin, M; Vásárhelyiné Perédi, K; Balázs, A; Blázovics, A; Simándi, B

2005-01-12

Antioxidant properties of marjoram (Origanum majorana L.) herb and extracts obtained with ethanol, n-hexane, and supercritical CO2 extraction are presented. Individual antioxidants, ursolic acid, carnosic acid, and carnosol, were quantified with high-performance liquid chromatography. The effects of different parameters (temperature and pressure) of high-pressure extraction on the yield of carnosol were studied. Furthermore, two marjoram herbs from Hungary and Egypt were compared measuring hydrogen-donating abilities with 1,1-diphenyl-2-picrylhydrazyl by spectrophotometric and the total scavenger capacities by chemiluminometric methods from the aqueous extracts of the herbs. The antioxidant activities of the solvent extracts were performed using the Rancimat method. The Egyptian herb and its extracts possessed better antioxidant activities than Hungarian ones. Applying supercritical CO2 extraction, the highest value of carnosol was obtained at 400 bar and 60 degrees C.

Fast ultrasound-assisted extraction of polar (phenols) and nonpolar (lipids) fractions in Heterotheca inuloides Cass.

PubMed

Ricárdez, O F Mijangos; Ruiz-Jiménez, J; Lagunez-Rivera, L; de Castro, M D Luque

2011-01-01

Heterotheca inuloides Cass., also known as "arnica", is used in traditional medicine in Mexico. Development of fast methods for the extraction of lipidic and phenolic fractions from arnica plants and their subsequent characterization. Ultrasound was applied to accelerate extraction of the target compounds from this plant and reduce the use of organic solvents as compared with conventional methods. Gas chromatography-ion trap mass spectrometry and liquid chromatography with diode-array detection were used for the characterization of the lipidic and phenolic fractions, respectively. Under optimal extraction conditions, 9 and 55 min were necessary to complete extraction of the lipidic and phenolic fractions, respectively. The fatty acids present at the highest concentrations in H. inuloides were eicosatetraenoic n3 (24.6 μg/g), cis-9-hexadecenoic n7 (23.1 μg/g), exacosanoic (22.7 μg/g) and cis-9-octadecenoic acid (21.3 μg/g), while the rest were in the range 7.6-1.3 μg/g. The most concentrated phenols were guaiacol (41.5 μg/g), catechin (38.7 μg/g), ellagic acid (35.9 μg/g), carbolic acid (24.2 μg/g) and p-coumaric acid (19.5 μg/g), while the rest were in the range 5.1-0.4 μg/g. Ultrasound reduces the time necessary to complete the extraction 160 and 26 times, the extraction volume 2.5 and 4 times, and increases the extraction efficiency 5 and 3 times for lipidic and phenolic fractions, respectively, in comparison with conventional extraction methods. In addition, the characterization of the lipidic and phenolic fractions constitutes a first approach to the H. inuloides metabolome. Copyright © 2011 John Wiley & Sons, Ltd.

Antibacterial activities and antioxidant capacity of Aloe vera

PubMed Central

2013-01-01

Background The aim of this study was to identify, quantify, and compare the phytochemical contents, antioxidant capacities, and antibacterial activities of Aloe vera lyophilized leaf gel (LGE) and 95% ethanol leaf gel extracts (ELGE) using GC-MS and spectrophotometric methods. Results Analytically, 95% ethanol is less effective than ethyl acetate/diethyl ether or hexane (in the case of fatty acids) extractions in separating phytochemicals for characterization purposes. However, although fewer compounds are extracted in the ELGE, they are approximately 345 times more concentrated as compared to the LGE, hence justifying ELGE use in biological efficacy studies in vivo. Individual phytochemicals identified included various phenolic acids/polyphenols, phytosterols, fatty acids, indoles, alkanes, pyrimidines, alkaloids, organic acids, aldehydes, dicarboxylic acids, ketones, and alcohols. Due to the presence of the antioxidant polyphenols, indoles, and alkaloids, the A. vera leaf gel shows antioxidant capacity as confirmed by ORAC and FRAP analyses. Both analytical methods used show the non-flavonoid polyphenols to contribute to the majority of the total polyphenol content. Three different solvents such as aqueous, ethanol, and acetone were used to extract the bioactive compounds from the leaves of A. vera to screen the antibacterial activity selected human clinical pathogens by agar diffusion method. The maximum antibacterial activities were observed in acetone extracts (12 ± 0.45, 20 ± 0.35, 20 ± 0.57, and 15 ± 0.38 nm) other than aqueous and ethanol extracts. Conclusion Due to its phytochemical composition, A. vera leaf gel may show promise in alleviating symptoms associated with/or prevention of cardiovascular diseases, cancer, neurodegeneration, and diabetes. PMID:23870710

A validated solid-liquid extraction method for the HPLC determination of polyphenols in apple tissues Comparison with pressurised liquid extraction.

PubMed

Alonso-Salces, Rosa M; Barranco, Alejandro; Corta, Edurne; Berrueta, Luis A; Gallo, Blanca; Vicente, Francisca

2005-02-15

A solid-liquid extraction procedure followed by reversed-phase high-performance liquid chromatography (RP-HPLC) coupled with a photodiode array detector (DAD) for the determination of polyphenols in freeze-dried apple peel and pulp is reported. The extraction step consists in sonicating 0.5g of freeze-dried apple tissue with 30mL of methanol-water-acetic acid (30:69:1, v/v/v) containing 2g of ascorbic acid/L, for 10min in an ultrasonic bath. The whole method was validated, concluding that it is a robust method that presents high extraction efficiencies (peel: >91%, pulp: >95%) and appropriate precisions (within day: R.S.D. (n = 5) <5%, and between days: R.S.D. (n = 5) <7%) at the different concentration levels of polyphenols that can be found in apple samples. The method was compared with one previously published, consisting in a pressurized liquid extraction (PLE) followed by RP-HPLC-DAD determination. The advantages and disadvantages of both methods are discussed.

Assessment of phenolic acid content and in vitro antiradical characteristics of hawthorn.

PubMed

Öztürk, Nilgün; Tunçel, Muzaffer

2011-06-01

The infusions and extracts obtained from leaves with flowers, fruit peel, and seed from hawthorn (Crataegus monogyna Jacq., Family Rosaceae) were subjected to evaluation as potential sources of antioxidant phytochemicals on the basis of their total content of phenolics, levels of phenolic acids, and in vitro antiradical activity. Total phenolic content of extracts was determined using the modified Folin-Ciocalteau method. Antioxidant activity was determined for phenolic extracts by a method involving the use of the free radical 2,2-diphenyl-1-picrylhydrazyl (DPPH). Phenolic acids containing extracts and infusions from hawthorn leaves, fruit peel, and seeds were obtained using different polarity solvents and separated by reverse-phase high-performance liquid chromatography, which enabled improved separation by the use of a C(18) column, an acidic mobile phase, and gradient elusion. The highest total phenolic content (343.54 mg of gallic acid equivalents/g) and the highest DPPH radical scavenging activity as the inhibition percentage (60.36%) were obtained in ethyl acetate extract from hawthorn leaves with flower. Also, the highest phenolic acid content was measured in the extracts of hawthorn leaves with flowers: protocathechuic (108-128 mg/100 g), p-hydroxy benzoic (141-468 mg/100 g), caffeic (137-3,580 mg/100 g), chlorogenic (925-4,637 mg/100 g), ferulic (3,363-3,462 mg/100 g), vanillic (214 mg/100 g), and syringic (126 mg/100 g) acids. The results indicate that hawthorn is a promising plant because of its high antioxidant activity.

Ultrasound-assisted extraction of gymnemic acids from Gymnema sylvestre leaves and its effect on insulin-producing RINm-5 F β cell lines.

PubMed

Sheoran, Sunita; Panda, Bibhu Prasad; Admane, Prasad S; Panda, Amulya Kumar; Wajid, Saima

2015-01-01

Gymnema sylvestre is an important anti-diabetic medicinal plant, hence it is necessary to study the effective extraction of its active medicinal components. To develop an efficient ultrasound-assisted extraction method for anti-diabetic gymnemic acids from Gymnema sylvestre leaves and measure their effect on insulin-producing RINm-5 F β cells. Box-Behnken's design and response surface methodology was applied to the ultrasound-assisted extraction of gymnemic acids from Gymnema sylvestre leaves. Analysis of gymnemic acids was carried out by high-performance thin-layer chromatography by converting total gymnemic acids into gymnemagenin by alkali hydrolysis. Effects of extracts on insulin production were tested on cultured, insulin-producing RINm-5 F β cell lines. The point prediction tool of the design expert software predicted 397.9 mg gymnemic acids per gram of the defatted G. sylvestre leaves using ultrasound-assisted extraction, with ethanol at 60 °C for 30 min. The predicted condition shows 93.34% validity under experimental conditions. The ultrasound-assisted extract caused up to about four times more insulin production from RINm-5 F β cells than extracts obtained from Soxhlet extraction. Response surface methodology was successfully used to improve the extraction of gymnemic acids from G. sylvestre leaves. The ultrasound-assisted extraction process may be a better alternative to prepare such herbal extracts because it saves time and may prevent excess degradation of the target analytes. Copyright © 2014 John Wiley & Sons, Ltd.

Focused microwave-assisted solvent extraction and HPLC determination of effective constituents in Eucommia ulmodies Oliv. (E. ulmodies).

PubMed

Li, Hui; Chen, Bo; Zhang, Zhaohui; Yao, Shouzhuo

2004-06-17

A new focused microwave-assisted solvent extraction method using water as solvent has been developed for leaching geniposidic and chlorogenic acids from Eucommia ulmodies Oliv. The extraction procedures were optimized using a two indexes orthogonal experimental design and graphical analysis, by varying irradiation time, solvent volume, solvent composition and microwave power. The optimum extraction conditions were obtained: for geniposidic acid, 50% micorwave power, 40s irradiation, and 80% (v/v) aqueous methanol as extraction solvent (20mlg(-1) sample); and for chlorogenic acid, 50% micorwave power, 30s irradiation, and 20% aqueous methanol (20mlg(-1) sample). The composition of the extraction solvent was optimized and can be directly used as the mobile phase in the HPLC separation. Quantification of organic acids was done by HPLC at room temperature using Spherigel C(18) chromatographic column (250 mm x4.6 mm , i.d. 5mum), the methanol:water:acetic acid (20:80:1.0, v/v) mobile phase and UV detection at 240nm. The R.S.D. of the extraction process for geniposidic and chlorogenic acid were 3.8 and 4.1%, respectively.

Injection port derivatization following ion-pair hollow fiber-protected liquid-phase microextraction for determining acidic herbicides by gas chromatography/mass spectrometry.

PubMed

Wu, Jingming; Lee, Hian Kee

2006-10-15

Injection port derivatization following ion-pair hollow fiber-protected liquid-phase microextraction (LPME) for the trace determination of acidic herbicides (2,4-dichlorobenzoic acid, 2,4-dichlorophenoxyacetic acid, 2-(2,4-dichlorophenoxy)propionic acid, 3,5-dichlorobenzoic acid, 2-(2,4,5-trichlorophenoxy)propionic acid) in aqueous samples by gas chromatography/mass spectrometry (GC/MS) was developed. Prior to GC injection port derivatization, acidic herbicides were converted into their ion-pair complexes with tetrabutylammonium chloride in aqueous samples and then extracted by 1-octanol impregnated in the hollow fiber. Upon injection, ion pairs of acidic herbicides were quantitatively derivatized to their butyl esters in the GC injection port. Thus, several parameters related to the derivatization process (i.e., injection temperature, purge-off time) were evaluated, and main parameters affecting the hollow fiber-protected LPME procedure such as extraction organic solvent, ion-pair reagent type, pH of aqueous medium, concentration of ion-pair reagent, sodium chloride concentration added to the aqueous medium, stirring speed, and extraction time profile, optimized. At the selected extraction and derivatization conditions, no matrix effects were observed. This method proved good repeatability (RSDs <12.3%, n = 6) and good linearity (r2 > or = 0.9939) for spiked deionized water samples for five analytes. The limits of detection were in the range of 0.51-13.7 ng x L(-1) (S/N =3) under GC/MS selected ion monitoring mode. The results demonstrated that injection port derivatization following ion-pair hollow fiber-protected LPME was a simple, rapid, and accurate method for the determination of trace acidic herbicides from aqueous samples. In addition, this method proved to be environmentally friendly since it completely avoided open derivatization with potentially hazardous reagents.

Ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME)-a fast new approach to measure phthalate metabolites in nails.

PubMed

Alves, Andreia; Vanermen, Guido; Covaci, Adrian; Voorspoels, Stefan

2016-09-01

A new, fast, and environmentally friendly method based on ultrasound assisted extraction combined with dispersive liquid-liquid microextraction (US-DLLME) was developed and optimized for assessing the levels of seven phthalate metabolites (including the mono(ethyl hexyl) phthalate (MEHP), mono(2-ethyl-5-hydroxyhexyl) phthalate (5-OH-MEHP), mono(2-ethyl-5-oxohexyl) phthalate (5-oxo-MEHP), mono-n-butyl phthalate (MnBP), mono-isobutyl phthalate (MiBP), monoethyl phthalate (MEP), and mono-benzyl phthalate (MBzP)) in human nails by UPLC-MS/MS. The optimization of the US-DLLME method was performed using a Taguchi combinatorial design (L9 array). Several parameters such as extraction solvent, solvent volume, extraction time, acid, acid concentration, and vortex time were studied. The optimal extraction conditions achieved were 180 μL of trichloroethylene (extraction solvent), 2 mL trifluoroacetic acid in methanol (2 M), 2 h extraction and 3 min vortex time. The optimized method had a good precision (6-17 %). The accuracy ranged from 79 to 108 % and the limit of method quantification (LOQm) was below 14 ng/g for all compounds. The developed US-DLLME method was applied to determine the target metabolites in 10 Belgian individuals. Levels of the analytes measured in nails ranged between <12 and 7982 ng/g. The MEHP, MBP isomers, and MEP were the major metabolites and detected in every sample. Miniaturization (low volumes of organic solvents used), low costs, speed, and simplicity are the main advantages of this US-DLLME based method. Graphical Abstract Extraction and phase separation of the US-DLLME procedure.

Solvent and process for recovery of hydroxide from aqueous mixtures

DOEpatents

Moyer, Bruce A.; Chambliss, C. Kevin; Bonnesen, Peter V.; Keever, Tamara J.

2001-01-01

Hydroxide values and associated alkali metal may be recovered from alkaline aqueous solutions using classes of fluorinated alcohols in a water immiscible solvent. The alcohols are characterized by fluorine substituents which are proximal to the acidic alcohol protons and are located to adjust the acidity of the extractant and the solubility of the extractant in the solvent. A method for stripping the extractant and solvent to regenerate the extractant and purified aqueous hydroxide solution is described.

Development, validation and evaluation of an analytical method for the determination of monomeric and oligomeric procyanidins in apple extracts.

PubMed

Hollands, Wendy J; Voorspoels, Stefan; Jacobs, Griet; Aaby, Kjersti; Meisland, Ane; Garcia-Villalba, Rocio; Tomas-Barberan, Francisco; Piskula, Mariusz K; Mawson, Deborah; Vovk, Irena; Needs, Paul W; Kroon, Paul A

2017-04-28

There is a lack of data for individual oligomeric procyanidins in apples and apple extracts. Our aim was to develop, validate and evaluate an analytical method for the separation, identification and quantification of monomeric and oligomeric flavanols in apple extracts. To achieve this, we prepared two types of flavanol extracts from freeze-dried apples; one was an epicatechin-rich extract containing ∼30% (w/w) monomeric (-)-epicatechin which also contained oligomeric procyanidins (Extract A), the second was an oligomeric procyanidin-rich extract depleted of epicatechin (Extract B). The parameters considered for method optimisation were HPLC columns and conditions, sample heating, mass of extract and dilution volumes. The performance characteristics considered for method validation included standard linearity, method sensitivity, precision and trueness. Eight laboratories participated in the method evaluation. Chromatographic separation of the analytes was best achieved utilizing a Hilic column with a binary mobile phase consisting of acidic acetonitrile and acidic aqueous methanol. The final method showed linearity for epicatechin in the range 5-100μg/mL with a correlation co-efficient >0.999. Intra-day and inter-day precision of the analytes ranged from 2 to 6% and 2 to 13% respectively. Up to dp3, trueness of the method was >95% but decreased with increasing dp. Within laboratory precision showed RSD values <5 and 10% for monomers and oligomers, respectively. Between laboratory precision was 4 and 15% (Extract A) and 7 and 30% (Extract B) for monomers and oligomers, respectively. An analytical method for the separation, identification and quantification of procyanidins in an apple extract was developed, validated and assessed. The results of the inter-laboratory evaluation indicate that the method is reliable and reproducible. Copyright © 2017. Published by Elsevier B.V.

Experimental design for extraction and quantification of phenolic compounds and organic acids in white "Vinho Verde" grapes.

PubMed

Dopico-García, M S; Valentão, P; Guerra, L; Andrade, P B; Seabra, R M

2007-01-30

An experimental design was applied for the optimization of extraction and clean-up processes of phenolic compounds and organic acids from white "Vinho Verde" grapes. The developed analytical method consisted in two steps: first a solid-liquid extraction of both phenolic compounds and organic acids and then a clean-up step using solid-phase extraction (SPE). Afterwards, phenolic compounds and organic acids were determined by high-performance liquid chromatography (HPLC) coupled to a diode array detector (DAD) and HPLC-UV, respectively. Plackett-Burman design was carried out to select the significant experimental parameters affecting both the extraction and the clean-up steps. The identified and quantified phenolic compounds were: quercetin-3-O-glucoside, quercetin-3-O-rutinoside, kaempferol-3-O-rutinoside, isorhamnetin-3-O-glucoside, quercetin, kaempferol and epicatechin. The determined organic acids were oxalic, citric, tartaric, malic, shikimic and fumaric acids. The obtained results showed that the most important variables were the temperature (40 degrees C) and the solvent (acid water at pH 2 with 5% methanol) for the extraction step and the type of sorbent (C18 non end-capped) for the clean-up step.

Nucleic acid purification from plants, animals and microbes in under 30 seconds

PubMed Central

Zou, Yiping; Wang, Yuling; Wee, Eugene; Turni, Conny; Blackall, Patrick J.; Trau, Matt; Botella, Jose Ramon

2017-01-01

Nucleic acid amplification is a powerful molecular biology tool, although its use outside the modern laboratory environment is limited due to the relatively cumbersome methods required to extract nucleic acids from biological samples. To address this issue, we investigated a variety of materials for their suitability for nucleic acid capture and purification. We report here that untreated cellulose-based paper can rapidly capture nucleic acids within seconds and retain them during a single washing step, while contaminants present in complex biological samples are quickly removed. Building on this knowledge, we have successfully created an equipment-free nucleic acid extraction dipstick methodology that can obtain amplification-ready DNA and RNA from plants, animals, and microbes from difficult biological samples such as blood and leaves from adult trees in less than 30 seconds. The simplicity and speed of this method as well as the low cost and availability of suitable materials (e.g., common paper towelling), means that nucleic acid extraction is now more accessible and affordable for researchers and the broader community. Furthermore, when combined with recent advancements in isothermal amplification and naked eye DNA visualization techniques, the dipstick extraction technology makes performing molecular diagnostic assays achievable in limited resource settings including university and high school classrooms, field-based environments, and developing countries. PMID:29161268

THE SOLVENT EXTRACTION OF NITROSYLRUTHENIUM BY TRILAURYLAMINE IN NITRATE SYSTEM. Summary Report for the Period, July 1, 1960 to March 31, 1962

DOE Office of Scientific and Technical Information (OSTI.GOV)

Skavdahl, R.E.; Mason, E.A.

1962-06-01

An investigation of the solvent extraction characteristics of the nitro and nitrato complexes of nitrosylruthenium in nitric acid- sodium nitrate aqueous media was conducted. As the organic extractant phase, a solution of trilaurylamine (TLA) in toluene was utilized. In addition to the usual process parameter variation tyne of experiment, a rapid dilution type of experiment was used extensively to determine qualitative and semiquantitative results regarding the degree of extractability and concentration of the more extractable species of the nitrato complexes of nitrosylruthenium. It was found that the acids of the tetra-nitrato and pentanitrato complexes were the more extractable species formore » that set of complexes and that the acid of the penta-nitrato complex was the more extractable of the two. It was observed that for freshly prepared solutions, the dinitro complex of nitrosylruthenium was much more extractable than the gross nitrato complexes solutions. Nitro complexes in general, and the dinitro complex in particular, may be the controlling agent in ruthenium decontamination of spent nuclear fuel processed by solvent extraction methods. The experimental results from both sets of complexes could be more meaningfully correlated on the basis of unbound nitric acid concentration in the organic phase than on the basis of nitric acid concentration in the aqueous phase. The extraction of nitric acid by TLA from nitric acid-sodium nitrate aqueous solutions was investigated and the results correlated on the basis of activity of the undissociated nitric acid in the aqueous phase. (auth)« less

SOLVENT EXTRACTION PROCESS FOR SEPARATING URANIUM AND PLUTONIUM FROM AQUEOUS ACIDIC SOLUTIONS OF NEUTRON IRRADIATED URANIUM

DOEpatents

Bruce, F.R.

1962-07-24

A solvent extraction process was developed for separating actinide elements including plutonium and uranium from fission products. By this method the ion content of the acidic aqueous solution is adjusted so that it contains more equivalents of total metal ions than equivalents of nitrate ions. Under these conditions the extractability of fission products is greatly decreased. (AEC)

Extraction Behaviors of Heavy Rare Earths with Organophosphoric Extractants: The Contribution of Extractant Dimer Dissociation, Acid Ionization, and Complexation. A Quantum Chemistry Study.

PubMed

Jing, Yu; Chen, Ji; Chen, Li; Su, Wenrou; Liu, Yu; Li, Deqian

2017-03-30

Heavy rare earths (HREs), namely Ho 3+ , Er 3+ , Tm 3+ , Yb 3+ and Lu 3+ , are rarer and more exceptional than light rare earths, due to the stronger extraction capacity for 100 000 extractions. Therefore, their incomplete stripping and high acidity of stripping become problems for HRE separation by organophosphoric extractants. However, the theories of extractant structure-performance relationship and molecular design method of novel HRE extractants are still not perfect. Beyond the coordination chemistry of the HRE-extracted complex, the extractant dimer dissociation, acid ionization, and complexation behaviors can be crucial to HRE extraction and reactivity of ionic species for understanding and further improving the extraction performance. To address the above issues, three primary fundamental processes, including extractant dimer dissociation, acid ionization, and HRE complexation, were identified and investigated systematically. The intrinsic extraction performances of HRE cations with four acidic organophosphoric extractants (P507, P204, P227 and Cyanex 272) were studied by using relativistic energy-consistent 4f core pseudopotentials, combined with density functional theory and a solvation model. Four acidic organophosphoric extractants have been qualified quantitatively from microscopic structures to chemical properties. It has been found that the Gibbs free energy changes of the overall extraction process (sequence: P204 > P227 > P507 > Cyanex 272) and their differences as a function of HREs (sequence: Ho/Er > Er/Tm > Tm/Yb > Yb/Lu) are in good agreement with the experimental maximum extraction capacities and separation factors. These results could provide an important approach to evaluate HRE extractants by the comprehensive consideration of dimer dissociation, acid ionization, and complexation processes. This paper also demonstrates the importance of the P-O bond, the P-C bond, isomer substituent, and solvation effects on the structure-performance relationship that can be used to guide molecular designs of HRE extraction in future.

Improving green enrichment of virgin olive oil by oregano. Effects on antioxidants.

PubMed

Peñalvo, Gregorio Castañeda; Robledo, Virginia Rodríguez; Callado, Carolina Sánchez-Carnerero; Santander-Ortega, M J; Castro-Vázquez, L; Lozano, M Victoria; Arroyo-Jiménez, M M

2016-04-15

This work is about improvement of a maceration method in order to achieve a green process for the enrichment of virgin olive oil (VOO) with natural antioxidants, specifically from oregano leaves. This goal was accomplished after evaluating different mechanical methods, i.e. magnetic stirring, sonication, vertical stirring and sonication in combination with vertical stirring, for promoting the extraction of the antioxidants from oregano. The results obtained indicated that the best extraction procedure was vertical stirring at 1000 r.p.m. for 3 h. Therefore, these conditions were selected to enrich VOO with phenolic acids (mainly rosmarinic acid) and endogenous antioxidants (o-coumaric and vanillic acids), and further determine their stability at room temperature or under temperature stress (50°C) during 45 days. Quantitative analysis of rosmarinic, o-coumaric and vanillic acids was carried out by an off-line, solid phase extraction, capillary zone, electrophoresis method combined with diode-array detector (SPE-CE-DAD). Copyright © 2015 Elsevier Ltd. All rights reserved.

Method for the recovery of actinide elements from nuclear reactor waste

DOEpatents

Horwitz, E. Philip; Delphin, Walter H.; Mason, George W.

1979-01-01

A process for partitioning and recovering actinide values from acidic waste solutions resulting from reprocessing of irradiated nuclear fuels by adding hydroxylammonium nitrate and hydrazine to the waste solution to adjust the valence of the neptunium and plutonium values in the solution to the +4 oxidation state, thus forming a feed solution and contacting the feed solution with an extractant of dihexoxyethyl phosphoric acid in an organic diluent whereby the actinide values, most of the rare earth values and some fission product values are taken up by the extractant. Separation is achieved by contacting the loaded extractant with two aqueous strip solutions, a nitric acid solution to selectively strip the americium, curium and rare earth values and an oxalate solution of tetramethylammonium hydrogen oxalate and oxalic acid or trimethylammonium hydrogen oxalate to selectively strip the neptunium, plutonium and fission product values. Uranium values remain in the extractant and may be recovered with a phosphoric acid strip. The neptunium and plutonium values are recovered from the oxalate by adding sufficient nitric acid to destroy the complexing ability of the oxalate, forming a second feed, and contacting the second feed with a second extractant of tricaprylmethylammonium nitrate in an inert diluent whereby the neptunium and plutonium values are selectively extracted. The values are recovered from the extractant with formic acid.

Process for the extraction of technetium from uranium

DOEpatents

Gong, Cynthia-May S.; Poineau, Frederic; Czerwinski, Kenneth R.

2010-12-21

A spent fuel reprocessing method contacts an aqueous solution containing Technetium(V) and uranyl with an acidic solution comprising hydroxylamine hydrochloride or acetohydroxamic acid to reduce Tc(V) to Tc(II, and then extracts the uranyl with an organic phase, leaving technetium(II) in aqueous solution.

A simple and accurate HPLC method for fecal bile acid profile in healthy and cirrhotic subjects: validation by GC-MS and LC-MS[S

PubMed Central

Kakiyama, Genta; Muto, Akina; Takei, Hajime; Nittono, Hiroshi; Murai, Tsuyoshi; Kurosawa, Takao; Hofmann, Alan F.; Pandak, William M.; Bajaj, Jasmohan S.

2014-01-01

We have developed a simple and accurate HPLC method for measurement of fecal bile acids using phenacyl derivatives of unconjugated bile acids, and applied it to the measurement of fecal bile acids in cirrhotic patients. The HPLC method has the following steps: 1) lyophilization of the stool sample; 2) reconstitution in buffer and enzymatic deconjugation using cholylglycine hydrolase/sulfatase; 3) incubation with 0.1 N NaOH in 50% isopropanol at 60°C to hydrolyze esterified bile acids; 4) extraction of bile acids from particulate material using 0.1 N NaOH; 5) isolation of deconjugated bile acids by solid phase extraction; 6) formation of phenacyl esters by derivatization using phenacyl bromide; and 7) HPLC separation measuring eluted peaks at 254 nm. The method was validated by showing that results obtained by HPLC agreed with those obtained by LC-MS/MS and GC-MS. We then applied the method to measuring total fecal bile acid (concentration) and bile acid profile in samples from 38 patients with cirrhosis (17 early, 21 advanced) and 10 healthy subjects. Bile acid concentrations were significantly lower in patients with advanced cirrhosis, suggesting impaired bile acid synthesis. PMID:24627129

Determination of perfluoroalkyl carboxylic, sulfonic, and phosphonic acids in food.

PubMed

Ullah, Shahid; Alsberg, Tomas; Vestergren, Robin; Berger, Urs

2012-11-01

A sensitive and accurate method was developed and validated for simultaneous analysis of perfluoroalkyl carboxylic acids, sulfonic acids, and phosphonic acids (PFPAs) at low picograms per gram concentrations in a variety of food matrices. The method employed extraction with acetonitrile/water and cleanup on a mixed-mode co-polymeric sorbent (C8 + quaternary amine) using solid-phase extraction. High-performance liquid chromatographic separation was achieved on a C18 column using a mobile phase gradient containing 5 mM 1-methyl piperidine for optimal chromatographic resolution of PFPAs. A quadrupole time-of-flight high-resolution mass spectrometer operating in negative ion mode was used as detector. Method detection limits were in the range of 0.002 to 0.02 ng g(-1) for all analytes. Sample preparation (extraction and cleanup) recoveries at a spiking level of 0.1 ng g(-1) to a baby food composite were in the range of 59 to 98 %. A strong matrix effect was observed in the analysis of PFPAs in food extracts, which was tentatively assigned to sorption of PFPAs to the injection vial in the solvent-based calibration standard. The method was successfully applied to a range of different food matrices including duplicate diet samples, vegetables, meat, and fish samples.

Rapid Determination of Two Triterpenoid Acids in Chaenomelis Fructus Using Supercritical Fluid Extraction On-line Coupled with Supercritical Fluid Chromatography.

PubMed

Zhang, Xiaotian; Ji, Feng; Li, Yueqi; He, Tian; Han, Ya; Wang, Daidong; Lin, Zongtao; Chen, Shizhong

2018-01-01

In this study, an on-line supercritical fluid extraction (SFE) and supercritical fluid chromatography (SFC) method was developed for the rapid determination of oleanoic acid and ursolic acid in Chaenomelis Fructus. After optimization of the conditions, the two triterpenoid acids was obtained by SFE using 20% methanol as a modifier at 35°C in 8 min. They were resolved on a Shim-pack UC-X Diol column (4.6 × 150 mm, 3 μm) in 14 min (0 - 10 min, 5 - 10%; 10 - 14 min, 10% methanol in CO 2 ) with a backpressure of 15 MPa at 40°C. The on-line SFE-SFC method could be completed within 40 min (10.79 mg/g dry plant, R s = 2.36), while the ultrasound-assisted extraction and HPLC method required at least 90 min (3.55 mg/g dry plant, R s = 1.92). This on-line SFE-SFC method is powerful to simplify the pre-processing and quantitative analysis of natural products.

An Effective Method to Detect Volatile Intermediates Generated in the Bioconversion of Coal to Methane by Gas Chromatography-Mass Spectrometry after In-Situ Extraction Using Headspace Solid-Phase Micro-Extraction under Strict Anaerobic Conditions.

PubMed

Liu, Jianmin; Wang, Baoyu; Tai, Chao; Wu, Li; Zhao, Han; Guan, Jiadong; Chen, Linyong

2016-01-01

Bioconversion of coal to methane has gained increased attention in recent decades because of its economic and environmental advantages. However, the mechanism of this process is difficult to study in depth, partly because of difficulties associated with the analysis of intermediates generated in coal bioconversion. In this investigation, we report on an effective method to analyze volatile intermediates generated in the bioconversion of coal under strict anaerobic conditions. We conduct in-situ extraction of intermediates using headspace solid-phase micro-extraction followed by detection by gas chromatography-mass spectrometry. Bioconversion simulation equipment was modified and combined with a solid-phase micro-extraction device. In-situ extraction could be achieved by using the combined units, to avoid a breakdown in anaerobic conditions and to maintain the experiment continuity. More than 30 intermediates were identified qualitatively in the conversion process, and the variation in trends of some typical intermediates has been discussed. Volatile organic acids (C2-C7) were chosen for a quantitative study of the intermediates because of their importance during coal bioconversion to methane. Fiber coating, extraction time, and solution acidity were optimized in the solid-phase micro-extraction procedure. The pressure was enhanced during the bioconversion process to investigate the influence of headspace pressure on analyte extraction. The detection limits of the method ranged from 0.0006 to 0.02 mmol/L for the volatile organic acids and the relative standard deviations were between 4.6% and 11.5%. The volatile organic acids (C2-C7) generated in the bioconversion process were 0.01-1.15 mmol/L with a recovery range from 80% to 105%. The developed method is useful for further in-depth research on the bioconversion of coal to methane.

An Effective Method to Detect Volatile Intermediates Generated in the Bioconversion of Coal to Methane by Gas Chromatography-Mass Spectrometry after In-Situ Extraction Using Headspace Solid-Phase Micro-Extraction under Strict Anaerobic Conditions

PubMed Central

Liu, Jianmin; Wang, Baoyu; Tai, Chao; Wu, Li; Zhao, Han; Guan, Jiadong; Chen, Linyong

2016-01-01

Bioconversion of coal to methane has gained increased attention in recent decades because of its economic and environmental advantages. However, the mechanism of this process is difficult to study in depth, partly because of difficulties associated with the analysis of intermediates generated in coal bioconversion. In this investigation, we report on an effective method to analyze volatile intermediates generated in the bioconversion of coal under strict anaerobic conditions. We conduct in-situ extraction of intermediates using headspace solid-phase micro-extraction followed by detection by gas chromatography-mass spectrometry. Bioconversion simulation equipment was modified and combined with a solid-phase micro-extraction device. In-situ extraction could be achieved by using the combined units, to avoid a breakdown in anaerobic conditions and to maintain the experiment continuity. More than 30 intermediates were identified qualitatively in the conversion process, and the variation in trends of some typical intermediates has been discussed. Volatile organic acids (C2–C7) were chosen for a quantitative study of the intermediates because of their importance during coal bioconversion to methane. Fiber coating, extraction time, and solution acidity were optimized in the solid-phase micro-extraction procedure. The pressure was enhanced during the bioconversion process to investigate the influence of headspace pressure on analyte extraction. The detection limits of the method ranged from 0.0006 to 0.02 mmol/L for the volatile organic acids and the relative standard deviations were between 4.6% and 11.5%. The volatile organic acids (C2–C7) generated in the bioconversion process were 0.01–1.15 mmol/L with a recovery range from 80% to 105%. The developed method is useful for further in-depth research on the bioconversion of coal to methane. PMID:27695055

Determination of Acid Herbicides Using Modified QuEChERS with Fast Switching ESI(+)/ESI(-) LC-MS/MS.

PubMed

Sack, Chris; Vonderbrink, John; Smoker, Michael; Smith, Robert E

2015-11-04

A method for the determination of 35 acid herbicides in food matrices was developed, validated, and implemented. It utilizes a modified QuEChERS extraction procedure coupled with quantitation by liquid chromatography tandem mass spectrometry (LC-MS/MS). The acid herbicides analyzed are all organic carboxylic acids, including the older chlorophenoxy acid herbicides such as 2,4-dichlorophenoxyacetic acid (2,4-D), dicamba, 4-chlorophenoxyacetic acid (4-CPA), quinclorac, and many of the newer imidazolinone herbicides such as imazethapyr and imazaquin. In the procedure, 10 mL of water is added to 5 g of sample and then extracted with 1% formic acid in acetonitrile for 1 min. The acetonitrile phase is salted out of the extract by adding sodium chloride and magnesium sulfate, followed by centrifugation. The acetonitrile is diluted 1:1 with water to enable quantitation by LC-MS/MS using fast switching between positive and negative electrospray ionization modes. The average recoveries for all the compounds except aminocyclopyrachlor were 95% with a precision of 8%. The method detection limits for all residues were less than 10 ng/g, and the correlation coefficients for the calibration curves was greater than 0.99 for all but two compounds tested. The method was used successfully for the quantitation of acid herbicides in the FDA's total diet study. The procedure proved to be accurate, precise, linear, sensitive, and rugged.

Development of an SPE/CE method for analyzing HAAs

USGS Publications Warehouse

Zhang, L.; Capel, P.D.; Hozalski, R.M.

2007-01-01

The haloacetic acid (HAA) analysis methods approved by the US Environmental Protection Agency involve extraction and derivatization of HAAs (typically to their methyl ester form) and analysis by gas chromatography (GC) with electron capture detection (ECD). Concerns associated with these methods include the time and effort of the derivatization process, use of potentially hazardous chemicals or conditions during methylation, poor recoveries because of low extraction efficiencies for some HAAs or matrix effects from sulfate, and loss of tribromoacetic acid because of decarboxylation. The HAA analysis method introduced here uses solid-phase extraction (SPE) followed by capillary electrophoresis (CE) analysis. The method is accurate, reproducible, sensitive, relatively safe, and easy to perform, and avoids the use of large amounts of solvent for liquid-liquid extraction and the potential hazards and hassles of derivatization. The cost of analyzing HAAs using this method should be lower than the currently approved methods, and utilities with a GC/ECD can perform the analysis in-house.

Ginger extract as green corrosion inhibitor of mild steel in hydrochloric acid solution

NASA Astrophysics Data System (ADS)

Fidrusli, A.; Suryanto; Mahmood, M.

2018-01-01

Ginger extract as corrosion inhibitor from natural resources was studied to prevent corrosion of mild steel in acid media. Ginger rhizome was extracted to produce green corrosion inhibitor (G-1) while ginger powder bought at supermarket was also extract to form green corrosion inhibitor (G-2). Effectiveness of inhibitor in preventing corrosion process of mild steel was studied in 1.0 M of hydrochloric acid. The experiment of weight loss method and polarization technique were conducted to measure corrosion rate and inhibition efficiency of mild steel in solution containing 1.0 M of hydrochloric acid with various concentration of inhibitor at room temperature. The results showed that, the rate of corrosion dropped from 8.09 mmpy in solution containing no inhibitor to 0.72 mmpy in solution containing 150g/l inhibitor while inhibition efficiency up to 91% was obtained. The polarization curve in polarization experiments shows that the inhibition efficiency is 86% with high concentration of inhibitor. The adsorption of ginger extract on the surface of mild steel was observed by using optical microscope and the characterization analysis was done by using pH measurement method. When high concentration of green inhibitor in the acid solution is used, the pH at the surface of steel is increasing.

Determination of free fatty acids in beer.

PubMed

Bravi, Elisabetta; Marconi, Ombretta; Sileoni, Valeria; Perretti, Giuseppe

2017-01-15

Free fatty acids (FFA) content of beer affects the ability to form a stable head of foam and plays an important role in beer staling. Moreover, the presence of saturated FAs is related sometimes to gushing problems in beer. The aim of this research was to validate an analytical method for the determination of FFAs in beer. The extraction of FFAs in beer was achieved via Liquid-Liquid Cartridge Extraction (LLCE), the FFAs extract was purified by Solid Phase Extraction (SPE), methylated by boron trifluoride in methanol, and injected into GC-FID system. The performance criteria demonstrate that this method is suitable for the analysis of medium and long chain FFAs in beer. The proposed method was tested on four experimental beers. Copyright © 2016 Elsevier Ltd. All rights reserved.

[Comparative study of different extraction methods and assays of tannins in some pteridophytes].

PubMed

Laurent, S

1975-10-01

Various processes of extraction and quantitative analysis of a condensed tannin in a plant extract, which also includes some chlorogenic acids, have been examined. 60% methanol, at 50 degrees C, proved the most efficient extraction solvent. Several methods of analysis have been tried. The measure of the colour intensity obtained by the action of sulphuric vanilline on flavanols cannot be used because it depends on the tannin condensation stage. It is impossible to separate tannin from chlorogenic acids using the methods of adsorption by skin or nylon powders, or precipitation by polyvinylpyrrolidone. Only paper chromatography, followed by the distinct elution of the various phenolic compounds, allows the tannin evaluation by subtraction; but owing to the variability of the results, many more experiments are necessary. Some other processes are being studied.

Automated extraction for the analysis of 11-nor-delta9-tetrahydrocannabinol-9-carboxylic acid (THCCOOH) in urine using a six-head probe Hamilton Microlab 2200 system and gas chromatography-mass spectrometry.

PubMed

Whitter, P D; Cary, P L; Leaton, J I; Johnson, J E

1999-01-01

An automated extraction scheme for the analysis of 11 -nor-delta9-tetrahydrocannabinol-9-carboxylic acid using the Hamilton Microlab 2200, which was modified for gravity-flow solid-phase extraction, has been evaluated. The Hamilton was fitted with a six-head probe, a modular valve positioner, and a peristaltic pump. The automated method significantly increased sample throughput, improved assay consistency, and reduced the time spent performing the extraction. Extraction recovery for the automated method was > 90%. The limit of detection, limit of quantitation, and upper limit of linearity were equivalent to the manual method: 1.5, 3.0, and 300 ng/mL, respectively. Precision at the 15-ng/mL cut-off was as follows: mean = 14.4, standard deviation = 0.5, coefficient of variation = 3.5%. Comparison of 38 patient samples, extracted by the manual and automated extraction methods, demonstrated the following correlation statistics: r = .991, slope 1.029, and y-intercept -2.895. Carryover was < 0.3% at 1000 ng/mL. Aliquoting/extraction time for the automated method (48 urine samples) was 50 min, and the manual procedure required approximately 2.5 h. The automated aliquoting/extraction method on the Hamilton Microlab 2200 and its use in forensic applications are reviewed.

Central composite design parameterization of microalgae/cyanobacteria co-culture pretreatment for enhanced lipid extraction using an external clamp-on ultrasonic transducer.

PubMed

Ellison, Candice R; Overa, Sean; Boldor, Dorin

2018-05-19

Lipids extracted from algal biomass could provide an abundant, rapidly growing, high yield feedstock for bio-diesel and other green fuels to supplement current fossil-based sources. Ultrasound pretreatment is a mechanical cell disruption method that has been shown to enhance lipid recovery from algae due to cavitation effects that disrupt algae cell walls. In this study, a locally grown mixture of Chlorella vulgaris/Cyanobacteria leptolyngbya was sonicated in an ultrasonic reactor with a clamp-on transducer prior to solvent lipid extraction. This configuration allows for a non-contact delivery method of ultrasonic energy with improved operational advantages (no fouling of transducer, continuous operation, and fully scalable design). A central composite design (CCD) was implemented to statistically analyze and evaluate the effect of ultrasonic power (350-750 W) and treatment time (5-30 min) on lipid yield. Lipid recovery was found to increase with both ultrasonic power and treatment time. Total lipid yields (on dry biomass basis) extracted via the Bligh and Dyer method from Chlorella vulgaris/cyanobacteria co-culture ranged from 8.3% for untreated algae to 16.9% for algae sonicated with 750 W power for 30 min, which corresponds to more than a doubling of lipid recovery due to ultrasound pretreatment. Increased power and treatment times were found to increase the degree of cell disruption as observed in the SEM and TEM images after ultrasonic pretreatment. Additionally, hexane (1:1 v/v) was evaluated as an alternative to the standard Bligh & Dyer (2:2:1.8 v/v/v chloroform/methanol/cell suspension) lipid extraction solvent system. On average, the Bligh and Dyer method extracted on average over twice the amount of lipids compared to hexane extraction. The lipid profile of the algae extracts indicates high concentrations of lauric acid (12:0), palmitic acid (16:0), stearic acid (18:0), oleic acid (18:1), and linoleic acid (18:2). This particular configuration of an ultrasonic system proved to be a viable method for the pretreatment of algae for enhanced lipid yields. Future research should focus on identifying alternative extraction solvents and expanding the range of treatment conditions to optimize the ultrasonic power and treatment times for maximum lipid recovery. Copyright © 2018 Elsevier B.V. All rights reserved.

Determination of aminopolycarboxylic acids in river water by solid-phase extraction on activated charcoal cartridges and gas chromatography with mass spectrometric detection. Method performance characteristics and estimation of the uncertainty.

PubMed

Jiménez, Juan J

2013-04-03

A new sample preparation procedure to determine aminopolycarboxylic acids (ethylenediaminetetraacetic acid, EDTA, nitrilotriacetic acid, NTA, diethylenetriaminepentaacetic acid, DTPA, and cyclohexanediaminetetraacetic acid, CDTA) in river water is described. The procedure consists of the solid-phase extraction of the aminopolycaroxyllic acids on activated charcoal cartridges after increasing the ionic strength and acidifying the sample. The extract was eluted with methanol and the analytes were methylated in presence of BF3/methanol to determine them by GC with mass spectrometric detection. Recoveries were higher than 90% with good repeatabilities and inter-day precision for concentrations close to quantification limits (about 10 μg L(-1)) and higher. It has been verified that the proposed method is robust according to the Youden and Steiner test and free of matrix effects arisen from the presence of organic matter and iron(III) as deduced from statistical tests. A bottom-up approach was followed to estimate the uncertainty of the measured concentration. At concentrations close to 10 μg L(-1) the most relevant step of the method is the calculus of the interpolated concentration which has a high value of relative standard uncertainty. Copyright © 2013 Elsevier B.V. All rights reserved.

Optimisation of Microwave-Assisted Extraction of Pomegranate (Punica granatum L.) Seed Oil and Evaluation 
of Its Physicochemical and Bioactive Properties.

PubMed

Çavdar, Hasene Keskin; Yanık, Derya Koçak; Gök, Uğur; Göğüş, Fahrettin

2017-03-01

Pomegranate seed oil was extracted in a closed-vessel high-pressure microwave system. The characteristics of the obtained oil, such as fatty acid composition, free fatty acidity, total phenolic content, antioxidant activity and colour, were compared to those of the oil obtained by cold solvent extraction. Response surface methodology was applied to optimise extraction conditions: power (176-300 W), time (5-20 min), particle size ( d =0.125-0.800 mm) and solvent to sample ratio (2:1, 6:1 and 10:1, by mass). The predicted highest extraction yield (35.19%) was obtained using microwave power of 220 W, particle size in the range of d =0.125-0.450 mm and solvent-to-sample ratio of 10:1 (by mass) in 5 min extraction time. Microwave-assisted solvent extraction (MASE) resulted in higher extraction yield than that of Soxhlet (34.70% in 8 h) or cold (17.50% in 8 h) extraction. The dominant fatty acid of pomegranate seed oil was punicic acid (86%) irrespective of the extraction method. Oil obtained by MASE had better physicochemical properties, total phenolic content and antioxidant activity than the oil obtained by cold solvent extraction.

Microwave-assisted extraction of pectin from cocoa peel

NASA Astrophysics Data System (ADS)

Sarah, M.; Hanum, F.; Rizky, M.; Hisham, M. F.

2018-02-01

Pectin is a polymer of d-galacturonate acids linked by β-1,4 glycosidic bond. This study isolates pectin from cocoa peel (Theobroma cacao) using citric acid as solvent by microwave-assisted extraction method. Cocoa peels (moisture content of 10%) with citric acid solution (pH of 1.5) irradiated by microwave energy at various microwave power (180, 300, 450 and 600 W) for 10, 15, 20, 25 and 30 minutes respectively. Pectin obtained from this study was collected and filtrated by adding 96% ethanol to precipitate the pectin. The best results obtained from extraction process using microwave power of 180 Watt for 30 minutes. This combination of power and time yielded 42.3% pectin with moisture content, ash content, weight equivalent, methoxyl content and galacturonate levels were 8.08%, 5%, 833.33 mg, 6.51% and 58,08%, respectively. The result finding suggested that microwave-assisted extraction method has a great potency on the commercial pectin production.

SOLVENT EXTRACTION PROCESS FOR PLUTONIUM

DOEpatents

Seaborg, G.T.

1959-04-14

The separation of plutonium from aqueous inorganic acid solutions by the use of a water immiscible organic extractant liquid is described. The plutonium must be in the oxidized state, and the solvents covered by the patent include nitromethane, nitroethane, nitropropane, and nitrobenzene. The use of a salting out agents such as ammonium nitrate in the case of an aqueous nitric acid solution is advantageous. After contacting the aqueous solution with the organic extractant, the resulting extract and raffinate phases are separated. The plutonium may be recovered by any suitable method.

Immobilization of microalgae cells in alginate facilitates isolation of DNA and RNA.

PubMed

Lopez, Blanca R; Hernandez, Juan-Pablo; Bashan, Yoav; de-Bashan, Luz E

2017-04-01

Isolation of nucleic acids from Chlorella is difficult, given the chemically complex nature of their cell walls and variable production of metabolites. Immobilization of microalgae in polymers adds additional difficulty. Here, we modified, amended, and standardized methods for isolation of nucleic acids and compared the yield of DNA and RNA from free-living and encapsulated microalgae C. sorokiniana. Isolation of nucleic acids from immobilized cells required two steps in dissolving the alginate matrix, releasing the cells, and mechanical disruption with glass beads. For DNA extraction, we used modified versions of a commercial kit along with the hexadecyltrimethylammonium bromide (CTAB) method. For RNA extraction, we used the commercial TRI reagent procedure and the CTAB-dithiotreitol method. Quantity and quality of nucleic acids in extracts varied with growth conditions, isolation procedures, and time of incubation of the original culture. There were consistently higher amounts of DNA and RNA in extracts from immobilized cells. Quantitatively, the modified procedure with the commercial Promega kit was the most reliable procedure for isolating DNA and a modified commercial TRI reagent procedure was the choice for isolating RNA. All four procedures eliminated proteins efficiently and had low levels of contamination from residual polysaccharides from the matrices and/or metabolites naturally produced by the microalgae. All DNA extracts under both growth conditions, time of incubation, and two isolation methods successfully amplified the 18S ribosomal RNA by PCR and quantitative reverse transcription (RT-qPCR). Copyright © 2017 Elsevier B.V. All rights reserved.

The Potency of White Rice (Oryza sativa), Black Rice (Oryza sativa L. indica), and Red Rice (Oryza nivara) as Antioxidant and Tyrosinase Inhibitor

NASA Astrophysics Data System (ADS)

Batubara, I.; Maharni, M.; Sadiah, S.

2017-04-01

Rice is known to have many beneficial biological activities and is often used as “bedak dingin”, a face powder. The content of vitamins, minerals, fiber, and several types of antioxidants, such as ferulic acid, phytic acid, tocopherol, and oryzanols [1-2] are predicted to be potential as a tyrosinase inhibitor. The purpose of this study is to determine the potency of extracts from there types of rice, namely white, red, and black rice as an antioxidant and tyrosinase inhibitor. The rice was extracted with three different solvents, n-hexane, ethyl acetate, and methanol. The results showed that the highest antioxidant activity using 1,1-diphenyl-2-picrylhydrazyl method was found in the methanol extract of black rice (IC50 290 μg/mL). Meanwhile, ethyl acetate extract of white rice has the highest antioxidant activity withphosphomolybdic acid method (41 mmol α-tocopherol equivalents/g sample). Thus, methanol extract of black rice and ethyl acetate extract of white rice are potential as an antioxidant. For tyrosinase inhibitor, n-hexane extract of red rice (IC50 3156 μg/mL) was the most active extract. The active component for radical scavenging is polar compound and for antioxidant by phosphomolybdate method is less polar compounds in black rice methanol extract based on TLC bioautogram. In conclusion, the black rice is the most potent in antioxidant while red rice is for tyrosinase inhibition.

Comparison of the Composition and Antioxidant Activities of Phenolics from the Fruiting Bodies of Cultivated Asian Culinary-Medicinal Mushrooms.

PubMed

Lin, Shaoling; Ching, Lai Tsz; Ke, Xinxin; Cheung, Peter Chi Keung

2016-01-01

The composition profile and the antioxidant properties of phenolics in water extracts obtained from the fresh fruiting bodies of 4 common cultivated Asian edible mushrooms-Agrocybe aegerita, Pleurotus ostreatus, P. eryngii, and Pholiota nameko were compared. The water extract from A. aegerita (AaE) had the highest total phenolic content (TPC) at 54.18 ± 0.27 gallic acid equivalents (μmol/L)/mg extract (P < 0.05), as measured by the Folin-Ciocalteu method, and consisted of the largest number (including gallic acid, protocatechuic acid, chlorogenic acid, ferulic acid, and sinapic acid) and total amounts of phenolic acids identified by Fourier transform-ion cyclotron resonance mass spectrometry. The water extract of Ph. nameko was found to have the second-highest TPC (43.55 ± 0.10 gallic acid equivalents [μmol/L]/mg extract), followed by the water extract of P. eryngii and the water extract of P. ostreatus (39.55 ± 0.25 and 39.02 ± 0.30 gallic acid equivalents/mg extract, respectively). The scavenging activities of the water extracts from these mushrooms were evaluated against 2,2-diphenyl-l-(2,4,6-trinitrophenyl) hydrazyl diphenylpicrylhydrazyl (DPPH), superoxide anion radicals, hydroxyl radicals, and hydrogen peroxide. Based on halfmaximal effective concentrations, AaE was more effective in scavenging hydrogen peroxide (<0.05), followed by DPPH (0.51 mg/mL), superoxide anion radicals (0.85 mg/mL) and hydroxyl radicals (5.94 mg/mL), then the other mushroom water extracts. The differences in the half-maximal effective concentrations of individual mushroom water extracts were probably the result of the different numbers and amounts of individual phenolic acids in the extracts. The antioxidant activities of the mushroom water extracts were correlated with their TPC. The strongest antioxidant properties of AaE were consistent with its highest TPC and with the largest number and amount of phenolics identified in the extract. These results indicated that cultivated edible mushrooms could be a potential source of natural antioxidants with free radical scavenging properties for application as a functional food ingredient.

Solid-phase extraction versus matrix solid-phase dispersion: Application to white grapes.

PubMed

Dopico-García, M S; Valentão, P; Jagodziñska, A; Klepczyñska, J; Guerra, L; Andrade, P B; Seabra, R M

2007-11-15

The use of matrix solid-phase dispersion (MSPD) was tested to, separately, extract phenolic compounds and organic acids from white grapes. This method was compared with a more conventional analytical method previously developed that combines solid liquid extraction (SL) to simultaneously extract phenolic compounds and organic acids followed by a solid-phase extraction (SPE) to separate the two types of compounds. Although the results were qualitatively similar for both techniques, the levels of extracted compounds were in general quite lower on using MSPD, especially for organic acids. Therefore, SL-SPE method was preferred to analyse white "Vinho Verde" grapes. Twenty samples of 10 different varieties (Alvarinho, Avesso, Asal-Branco, Batoca, Douradinha, Esganoso de Castelo Paiva, Loureiro, Pedernã, Rabigato and Trajadura) from four different locations in Minho (Portugal) were analysed in order to study the effects of variety and origin on the profile of the above mentioned compounds. Principal component analysis (PCA) was applied separately to establish the main sources of variability present in the data sets for phenolic compounds, organic acids and for the global data. PCA of phenolic compounds accounted for the highest variability (77.9%) with two PCs, enabling characterization of the varieties of samples according to their higher content in flavonol derivatives or epicatechin. Additionally, a strong effect of sample origin was observed. Stepwise linear discriminant analysis (SLDA) was used for differentiation of grapes according to the origin and variety, resulting in a correct classification of 100 and 70%, respectively.

Supercritical fluid extraction of 13-cis retinoic acid and its photoisomers from selected pharmaceutical dosage forms.

PubMed

Simmons, B R; Chukwumerije, O; Stewart, J T

1997-11-01

13-Cis retinoic acid (Accutane) was extracted from a cream, gel, capsule and beadlet dosage from using supercritical carbon dioxide modified with 5% methanol as the mobile phase. The pump pressure and the extraction chamber and restrictor temperature were experimentally optimized at 325 atm and 45 degrees C, respectively. A 2.5-min static and 5-min dynamic extraction time were used. The supercritical fluid extraction (SFE) eluent was trapped in methanol, injected into the high-performance liquid chromatographic (HPLC) system, and quantitated by ultraviolet detection at 360 nm. Application of the SFE method to spiked placebo dosage forms gave 13-cis retinoic acid recoveries of 98.8, 98.9, 98.8 and 100% for the cream, gel, capsule and beadlet, respectively, with R.S.D.s in the range 0.6-0.9% (n = 4). Inter-day percent error and precision of the extraction were 1.1-2.0 and 0.2-2.4% (n = 3), respectively, and intra-day percent error and precision were 1.0-3.0 and 0.3-2.1% (n = 8), respectively. Percent error and precision data for spiked celite samples in the 0.05-1.0 microgram ml-1 range were 0.59-4.75 and 1.8-2.1% (n = 3), respectively. The extraction method was applied to commercial 13-cis retinoic acid dosage forms and the results compared to unextracted samples. Linear regression analysis of concentration versus peak height gave a correlation coefficient of 0.9991 with a slope of 7.468 and a y-intercept of 0.1923. The percent error and precision data were 1.3-5.3 and 0.2-1.5% (n = 4), respectively. The photoisomers of 13-cis retinoic acid were also extracted with the method and recoveries of 90.4-92.4% with R.S.D.s of 1.5-3.4% were obtained (n = 4).

Two-step voltage dual electromembrane extraction: A new approach to simultaneous extraction of acidic and basic drugs.

PubMed

Asadi, Sakine; Nojavan, Saeed

2016-06-07

In the present work, acidic and basic drugs were simultaneously extracted by a novel method of high efficiency herein referred to as two-step voltage dual electromembrane extraction (TSV-DEME). Optimizing effective parameters such as composition of organic liquid membrane, pH values of donor and acceptor solutions, voltage and duration of each step, the method had its figures of merit investigated in pure water, human plasma, wastewater, and breast milk samples. Simultaneous extraction of acidic and basic drugs was done by applying potentials of 150 V and 400 V for 6 min and 19 min as the first and second steps, respectively. The model compounds were extracted from 4 mL of sample solution (pH = 6) into 20 μL of each acceptor solution (32 mM NaOH for acidic drugs and 32 mM HCL for basic drugs). 1-Octanol was immobilized within the pores of a porous hollow fiber of polypropylene, as the supported liquid membrane (SLM) for acidic drugs, and 2-ethyle hexanol, as the SLM for basic drugs. The proposed TSV-DEME technique provided good linearity with the resulting correlation coefficients ranging from 0.993 to 0.998 over a concentration range of 1-1000 ng mL(-1). The limit of detections of the drugs were found to range within 0.3-1.5 ng mL(-1), while the corresponding repeatability ranged from 7.7 to 15.5% (n = 4). The proposed method was further compared to simple dual electromembrane extraction (DEME), indicating significantly higher recoveries for TSV-DEME procedure (38.1-68%), as compared to those of simple DEME procedure (17.7-46%). Finally, the optimized TSV-DEME was applied to extract and quantify model compounds in breast milk, wastewater, and plasma samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Fluid extraction using carbon dioxide and organophosphorus chelating agents

DOEpatents

Smart, N.G.; Wai, C.M.; Lin, Y.; Kwang, Y.H.

1998-11-24

Methods for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical CO{sub 2}, and a chelating agent are described. The chelating agent forms a chelate with the species, the chelate being soluble in the fluid to allow removal of the species from the material. In preferred embodiments the extraction solvent is supercritical CO{sub 2} and the chelating agent comprises an organophosphorous chelating agent, particularly sulfur-containing organophosphorous chelating agents, including mixtures of chelating agents. Examples of chelating agents include monothiophosphinic acid, di-thiophosphinic acid, phosphine sulfite, phosphorothioic acid, and mixtures thereof. The method provides an environmentally benign process for removing metal and metalloids from industrial waste solutions, particularly acidic solutions. Both the chelate and the supercritical fluid can be regenerated and the contaminant species recovered to provide an economic, efficient process. 1 fig.

Fluid extraction using carbon dioxide and organophosphorus chelating agents

DOEpatents

Smart, Neil G.; Wai, Chien M.; Lin, Yuehe; Kwang, Yak Hwa

1998-01-01

Methods for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical CO.sub.2, and a chelating agent are described. The chelating agent forms a chelate with the species, the chelate being soluble in the fluid to allow removal of the species from the material. In preferred embodiments the extraction solvent is supercritical CO.sub.2 and the chelating agent comprises an organophosphorous chelating agent, particularly sulfur-containing organophosphorous chelating agents, including mixtures of chelating agents. Examples of chelating agents include monothiophosphinic acid, di-thiophosphinic acid, phosphine sulfite, phosphorothioic acid, and mixtures thereof. The method provides an environmentally benign process for removing metal and metalloids from industrial waste solutions, particularly acidic solutions. Both the chelate and the supercritical fluid can be regenerated and the contaminant species recovered to provide an economic, efficient process.

Comparative polyphenolic content and antioxidant activities of Genista tinctoria L. and Genistella sagittalis (L.) Gams (Fabaceae).

PubMed

Hanganu, Daniela; Olah, Neli Kinga; Benedec, Daniela; Mocan, Andrei; Crisan, Gianina; Vlase, Laurian; Popica, Iulia; Oniga, Ilioara

2016-01-01

The aim of this study was focused on the polyphenolic composition and antioxidant capacity of Genista tinctoria L. and Genistella sagittalis (L.) Gams. A qualitative and quantitative characterization of the main phenolic compounds from the extracts were carried out using a HPLC-MS method. The total polyphenolic and flavonoid content was spectrophotometrically determined. The antioxidant activity towards various radicals generated in different systems was evaluated usingDPPH bleaching method, Trolox equivalent antioxidant capacity assay (TEAC) and Oxygen radical absorbance capacity (ORAC), and all indicated that G. tinctoria extract was more antioxidant than G. sagittalis extract.That was in good agreement with the total polyphenolic and flavonoidic content.Chlorogenic acid, p-coumaric acid, isoquercitrin and apigenin were identified in bothspecies. Caffeic acid, ferulic acid, hyperoside, rutin, quercitrin and luteolin were found only in G. tinctoria, while quercetin was determined in G. sagittalis.

DNA extraction on bio-chip: history and preeminence over conventional and solid-phase extraction methods.

PubMed

Ayoib, Adilah; Hashim, Uda; Gopinath, Subash C B; Md Arshad, M K

2017-11-01

This review covers a developmental progression on early to modern taxonomy at cellular level following the advent of electron microscopy and the advancement in deoxyribonucleic acid (DNA) extraction for expatiation of biological classification at DNA level. Here, we discuss the fundamental values of conventional chemical methods of DNA extraction using liquid/liquid extraction (LLE) followed by development of solid-phase extraction (SPE) methods, as well as recent advances in microfluidics device-based system for DNA extraction on-chip. We also discuss the importance of DNA extraction as well as the advantages over conventional chemical methods, and how Lab-on-a-Chip (LOC) system plays a crucial role for the future achievements.

Antioxidant activity and total phenols from the methanolic extract of Miconia albicans (Sw.) Triana leaves.

PubMed

Pieroni, Laís Goyos; de Rezende, Fernanda Mendes; Ximenes, Valdecir Farias; Dokkedal, Anne Lígia

2011-11-10

Miconia is one of the largest genus of the Melastomataceae, with approximately 1,000 species. Studies aiming to describe the diverse biological activities of the Miconia species have shown promising results, such as analgesic, antimicrobial and trypanocidal properties. M. albicans leaves were dried, powdered and extracted to afford chloroformic and methanolic extracts. Total phenolic contents in the methanolic extract were determined according to modified Folin-Ciocalteu method. The antioxidant activity was measured using AAPH and DPPH radical assays. Chemical analysis was performed with the n-butanol fraction of the methanolic extract and the chloroformic extract, using different chromatographic techniques (CC, HPLC). The structural elucidation of compounds was performed using 500 MHz NMR and HPLC methods. The methanolic extract showed a high level of total phenolic contents; the results with antioxidant assays showed that the methanolic extract, the n-butanolic fraction and the isolated flavonoids from M. albicans had a significant scavenging capacity against AAPH and DPPH. Quercetin, quercetin-3-O-glucoside, rutin, 3-(E)-p-coumaroyl-α-amyrin was isolated from the n-butanolic fraction and α-amyrin, epi-betulinic acid, ursolic acid, epi-ursolic acid from the chloroformic extract. The results presented in this study demonstrate that M. albicans is a promising species in the search for biologically active compounds.

Electro-driven extraction of polar compounds using agarose gel as a new membrane: Determination of amino acids in fruit juice and human plasma samples.

PubMed

Sedehi, Samira; Tabani, Hadi; Nojavan, Saeed

2018-03-01

In this work, polypropylene hollow fiber was replaced by agarose gel in conventional electro membrane extraction (EME) to develop a novel approach. The proposed EME method was then employed to extract two amino acids (tyrosine and phenylalanine) as model polar analytes, followed by HPLC-UV. The method showed acceptable results under optimized conditions. This green methodology outperformed conventional EME, and required neither organic solvents nor carriers. The effective parameters such as the pH values of the acceptor and the donor solutions, the thickness and pH of the gel, the extraction voltage, the stirring rate, and the extraction time were optimized. Under the optimized conditions (acceptor solution pH: 1.5; donor solution pH: 2.5; agarose gel thickness: 7mm; agarose gel pH: 1.5; stirring rate of the sample solution: 1000rpm; extraction potential: 40V; and extraction time: 15min), the limits of detection and quantification were 7.5ngmL -1 and 25ngmL -1 , respectively. The extraction recoveries were between 56.6% and 85.0%, and the calibration curves were linear with correlation coefficients above 0.996 over a concentration range of 25.0-1000.0ngmL -1 for both amino acids. The intra- and inter-day precisions were in the range of 5.5-12.5%, and relative errors were smaller than 12.0%. Finally, the optimized method was successfully applied to preconcentrate, clean up, and quantify amino acids in watermelon and grapefruit juices as well as a plasma sample, and acceptable relative recoveries in the range of 53.9-84.0% were obtained. Copyright © 2017 Elsevier B.V. All rights reserved.

Methods of combined bioprocessing and related microorganisms, thermophilic and/or acidophilic enzymes, and nucleic acids encoding said enzymes

DOEpatents

Thompson, David N.; Apel, William A.; Thompson, Vicki S.; Ward, Thomas E.

2016-03-22

A genetically modified organism comprising: at least one nucleic acid sequence and/or at least one recombinant nucleic acid isolated from Alicyclobacillus acidocaldarius and encoding a polypeptide involved in at least partially degrading, cleaving, transporting, metabolizing, or removing polysaccharides, cellulose, lignocellulose, hemicellulose, lignin, starch, sugars, sugar oligomers, carbohydrates, complex carbohydrates, chitin, heteroxylans, glycosides, xylan-, glucan-, galactan-, or mannan-decorating groups; and at least one nucleic acid sequence and/or at least one recombinant nucleic acid encoding a polypeptide involved in fermenting sugar molecules to a product. Additionally, enzymatic and/or proteinaceous extracts may be isolated from one or more genetically modified organisms. The extracts are utilized to convert biomass into a product. Further provided are methods of converting biomass into products comprising: placing the genetically modified organism and/or enzymatic extracts thereof in fluid contact with polysaccharides, cellulose, lignocellulose, hemicellulose, lignin, starch, sugars, sugar oligomers, carbohydrates, complex carbohydrates, chitin, heteroxylans, glycosides, and/or xylan-, glucan-, galactan-, or mannan-decorating groups.

Methods of combined bioprocessing and related microorganisms, thermophilic and/or acidophilic enzymes, and nucleic acids encoding said enzymes

DOEpatents

Thompson, David N; Apel, William A; Thompson, Vicki S; Ward, Thomas E

2013-07-23

A genetically modified organism comprising: at least one nucleic acid sequence and/or at least one recombinant nucleic acid isolated from Alicyclobacillus acidocaldarius and encoding a polypeptide involved in at least partially degrading, cleaving, transporting, metabolizing, or removing polysaccharides, cellulose, lignocellulose, hemicellulose, lignin, starch, sugars, sugar oligomers, carbohydrates, complex carbohydrates, chitin, heteroxylans, glycosides, xylan-, glucan-, galactan-, or mannan-decorating groups; and at least one nucleic acid sequence and/or at least one recombinant nucleic acid encoding a polypeptide involved in fermenting sugar molecules to a product. Additionally, enzymatic and/or proteinaceous extracts may be isolated from one or more genetically modified organisms. The extracts are utilized to convert biomass into a product. Further provided are methods of converting biomass into products comprising: placing the genetically modified organism and/or enzymatic extracts thereof in fluid contact with polysaccharides, cellulose, lignocellulose, hemicellulose, lignin, starch, sugars, sugar oligomers, carbohydrates, complex carbohydrates, chitin, heteroxylans, glycosides, and/or xylan-, glucan-, galactan-, or mannan-decorating groups.

Methods of combined bioprocessing and related microorganisms, thermophilic and/or acidophilic enzymes, and nucleic acids encoding said enzymes

DOEpatents

Thompson, David N; Apel, William A; Thompson, Vicki S; Ward, Thomas E

2014-04-08

A genetically modified organism comprising: at least one nucleic acid sequence and/or at least one recombinant nucleic acid isolated from Alicyclobacillus acidocaldarius and encoding a polypeptide involved in at least partially degrading, cleaving, transporting, metabolizing, or removing polysaccharides, cellulose, lignocellulose, hemicellulose, lignin, starch, sugars, sugar oligomers, carbohydrates, complex carbohydrates, chitin, heteroxylans, glycosides, xylan-, glucan-, galactan-, or mannan-decorating groups; and at least one nucleic acid sequence and/or at least one recombinant nucleic acid encoding a polypeptide involved in fermenting sugar molecules to a product. Additionally, enzymatic and/or proteinaceous extracts may be isolated from one or more genetically modified organisms. The extracts are utilized to convert biomass into a product. Further provided are methods of converting biomass into products comprising: placing the genetically modified organism and/or enzymatic extracts thereof in fluid contact with polysaccharides, cellulose, lignocellulose, hemicellulose, lignin, starch, sugars, sugar oligomers, carbohydrates, complex carbohydrates, chitin, heteroxylans, glycosides, and/or xylan-, glucan-, galactan-, or mannan-decorating groups.

Direct quantitation of fatty acids present in bacteria and fungi: stability of the cyclopropane ring to chlorotrimethylsilane.

PubMed

Eras, Jordi; Oró, Robert; Torres, Mercè; Canela, Ramon

2008-07-09

The stability of the cyclopropane ring and the fatty acid composition of microbial cells were determined using chlorotrimethylsilane as reagent with three different conditions 80 degrees C for 1 h, 60 degrees C for 1 h, and 60 degrees C for 2 h. Chlorotrimethylsilane permits a simultaneous extraction and derivatization of fatty acids. A basic method was used as reference. The bacteria, Escherichia coli, Burkholderia cepacia, and Lactobacillus brevis, and fungi Aspergillus niger and Gibberella fujikuroi were used. The stability of the cyclopropane ring on acidic conditions was tested using the cyclopropanecarboxylic acid and a commercial mixture of bacteria fatty acid methyl esters (BAME). Fisher's least significant difference test showed significant differences among the methods. The method using chlorotrimethylsilane and 1-pentanol for 1 h at 80 degrees C gave the best results in cyclopropane, hydroxyl, and total fatty acid recoveries. This procedure allows the fast and easy one-step direct extraction derivatization.

Detection of naphthenic acids in fish exposed to commercial naphthenic acids and oil sands process-affected water.

PubMed

Young, R F; Orr, E A; Goss, G G; Fedorak, P M

2007-06-01

Naphthenic acids are a complex mixture of carboxylic acids that occur naturally in petroleum. During the extraction of bitumen from the oil sands in northeastern Alberta, Canada, naphthenic acids are released into the aqueous phase and these acids become the most toxic components in the process-affected water. Although previous studies have exposed fish to naphthenic acids or oil sands process-affected waters, there has been no analytical method to specifically detect naphthenic acids in fish. Here, we describe a qualitative method to specifically detect these acids. In 96-h static renewal tests, rainbow trout (Oncorhynchus mykiss) fingerlings were exposed to three different treatments: (1) fed pellets that contained commercial naphthenic acids (1.5mg g(-1) of food), (2) kept in tap water that contained commercial naphthenic acids (3mg l(-1)) and (3) kept in an oil sands process-affected water that contained 15mg naphthenic acids l(-1). Five-gram samples of fish were homogenized and extracted, then the mixture of free fatty acids and naphthenic acids was isolated from the extract using strong anion exchange chromatography. The mixture was derivatized and analyzed by gas chromatography-mass spectrometry. Reconstructed ion chromatograms (m/z=267) selectively detected naphthenic acids. These acids were present in each fish that was exposed to naphthenic acids, but absent in fish that were not exposed to naphthenic acids. The minimum detectable concentration was about 1microg naphthenic acids g(-1) of fish.

Simple and sensitive analysis of long-chain free fatty acids in milk by fluorogenic derivatization and high-performance liquid chromatography.

PubMed

Lu, Chi-Yu; Wu, Hsin-Lung; Chen, Su-Hwei; Kou, Hwang-Shang; Wu, Shou-Mei

2002-01-02

A highly sensitive high-performance liquid chromatography (HPLC) method is described for the simultaneous determination of some important saturated and unsaturated fatty acids in milk, including lauric (dodecanoic), myristic (tetradecanoic), palmitic (hexadecanoic), stearic (octadecanoic), palmitoleic (hexadecenoic), oleic (octadecenoic), and linoleic acids (octadecadienoic acids). The fatty acids were fluorogenically derivatized with 2-(2-naphthoxy)ethyl 2-(piperidino)ethanesulfonate (NOEPES) as their naphthoxyethyl derivatives. The resulting derivatives were separated by isocratic HPLC and monitored with a fluorometric detector (lambdaex = 235 nm, lambdaem = 350 nm). The fatty acids in milk were extracted with toluene, and the extract with the fatty acids was directly derivatized with NOEPES without solvent replacement. Determination of long-chain free fatty acids in milk is feasible by a standard addition method. A small amount of milk product, 10 microL, is sufficient for the analysis.

A METHOD FOR AUTOMATED ANALYSIS OF 10 ML WATER SAMPLES CONTAINING ACIDIC, BASIC, AND NEUTRAL SEMIVOLATILE COMPOUNDS LISTED IN USEPA METHOD 8270 BY SOLID PHASE EXTRACTION COUPLED IN-LINE TO LARGE VOLUME INJECTION GAS CHROMATOGRAPHY/MASS SPECTROMETRY

EPA Science Inventory

Data is presented showing the progress made towards the development of a new automated system combining solid phase extraction (SPE) with gas chromatography/mass spectrometry for the single run analysis of water samples containing a broad range of acid, base and neutral compounds...

Effects of oxidizing adulterants on detection of 11-nor-delta9-THC-9-carboxylic acid in urine.

PubMed

Paul, Buddha D; Jacobs, Aaron

2002-10-01

Bleach, nitrite, chromate, and hydrogen peroxide-peroxidase are effective urine adulterants used by the illicit drug users to conceal marijuana-positive results. Methods for detecting nitrite and chromate are available. Effects of other oxidizing agents that could possibly be used as adulterants and are difficult to detect or measure are presented in this report. Urine samples containing 40 ng/mL of 11-nor-delta9-THC-9-carboxylic acid (THC-acid) were treated with 10 mmol/L of commonly available oxidizing agents. Effects of horseradish peroxidase of activity 10 unit/mL and extracts from 2.5 g of red radish (Raphanus sativus, Radicula group), horseradish (Armoracia rusticana), Japanese radish (Raphanus sativus, Daikon group), and black mustard seeds (Brassica nigra), all with 10 mmol/L of hydrogen peroxide, were also examined. After 5 min, 16 h and 48 h of exposure at room temperature (23 degrees C) the specimens were tested by a gas chromatographic-mass spectrometric method for THC-acid. A control group treated with sodium hydrosulfite to reduce the oxidants, was also tested to investigate the effect of oxidizing agents on THC-acid in the extraction method. THC-acid was lost completely in the extraction method when treated with chromate, nitrite, oxone, and hydrogen peroxide/ferrous ammonium sulfate (Fenton's reagent). Some losses were also observed with persulfate and periodate (up to 25%). These oxidants, and other oxidizing agents like permanganate, periodate, peroxidase, and extracts from red radish, horseradish, Japanese radish and black mustard seeds destroyed most of the THC-acid (> 94%) within 48 h of exposure. Chlorate, perchlorate, iodate, and oxychloride under these conditions showed little or no effect. Complete loss was observed when THC-acid was exposed to 50 mmol/L of oxychloride for 48 h. Several oxidizing adulterants that are difficult to test by the present urine adulterant testing methods showed considerable effects on the destruction of THC-acid. The time and temperature for these effects were similar to those used by most laboratories to collect and test specimens. In several cases, the loss of THC-acid was > 94%.

Guava leaves polyphenolics-rich extract inhibits vital enzymes implicated in gout and hypertension in vitro

PubMed Central

Irondi, Emmanuel Anyachukwu; Agboola, Samson Olalekan; Oboh, Ganiyu; Boligon, Aline Augusti; Athayde, Margareth Linde; Shode, Francis O.

2016-01-01

Background/Aim: Elevated uric acid level, an index of gout resulting from the over-activity of xanthine oxidase (XO), increases the risk of developing hypertension. However, research has shown that plant-derived inhibitors of XO and angiotensin 1-converting enzyme (ACE), two enzymes implicated in gout and hypertension, respectively, can prevent or ameliorate both diseases, without noticeable side effects. Hence, this study characterized the polyphenolics composition of guava leaves extract and evaluated its inhibitory effect on XO and ACE in vitro. Materials and Methods: The polyphenolics (flavonoids and phenolic acids) were characterized using high-performance liquid chromatography (HPLC) coupled with diode array detection (DAD). The XO, ACE, and Fe2+-induced lipid peroxidation inhibitory activities, and free radicals (2,2-diphenylpicrylhydrazyl [DPPH]* and 2,2´-azino-bis-3-ethylbenzthiazoline-6-sulphonic [ABTS]*+) scavenging activities of the extract were determined using spectrophotometric methods. Results: Flavonoids were present in the extract in the order of quercetin > kaempferol > catechin > quercitrin > rutin > luteolin > epicatechin; while phenolic acids were in the order of caffeic acid > chlorogenic acid > gallic acids. The extract effectively inhibited XO, ACE and Fe2+-induced lipid peroxidation in a dose-dependent manner; having half-maximal inhibitory concentrations (IC50) of 38.24 ± 2.32 μg/mL, 21.06 ± 2.04 μg/mL and 27.52 ± 1.72 μg/mL against XO, ACE and Fe2+-induced lipid peroxidation, respectively. The extract also strongly scavenged DPPH* and ABTS*+. Conclusion: Guava leaves extract could serve as functional food for managing gout and hypertension and attenuating the oxidative stress associated with both diseases. PMID:27104032

Characterization of citrus pectin samples extracted under different conditions: influence of acid type and pH of extraction

PubMed Central

Kaya, Merve; Sousa, António G.; Crépeau, Marie-Jeanne; Sørensen, Susanne O.; Ralet, Marie-Christine

2014-01-01

Background and Aims Pectin is a complex macromolecule, the fine structure of which is influenced by many factors. It is used as a gelling, thickening and emulsifying agent in a wide range of applications, from food to pharmaceutical products. Current industrial pectin extraction processes are based on fruit peel, a waste product from the juicing industry, in which thousands of tons of citrus are processed worldwide every year. This study examines how pectin components vary in relation to the plant source (orange, lemon, lime, grapefruit) and considers the influence of extraction conditions on the chemical and macromolecular characteristics of pectin samples. Methods Citrus peel (orange, lemon, lime and grapefruit) from a commercial supplier was used as raw material. Pectin samples were obtained on a bulk plant scale (kilograms; harsh nitric acid, mild nitric acid and harsh oxalic acid extraction) and on a laboratory scale (grams; mild oxalic acid extraction). Pectin composition (acidic and neutral sugars) and physicochemical properties (molar mass and intrinsic viscosity) were determined. Key Results Oxalic acid extraction allowed the recovery of pectin samples of high molecular weight. Mild oxalic acid-extracted pectins were rich in long homogalacturonan stretches and contained rhamnogalacturonan I stretches with conserved side chains. Nitric acid-extracted pectins exhibited lower molecular weights and contained rhamnogalacturonan I stretches encompassing few and/or short side chains. Grapefruit pectin was found to have short side chains compared with orange, lime and lemon. Orange and grapefruit pectin samples were both particularly rich in rhamnogalacturonan I backbones. Conclusions Structural, and hence macromolecular, variations within the different citrus pectin samples were mainly related to their rhamnogalacturonan I contents and integrity, and, to a lesser extent, to the length of their homogalacturonan domains. PMID:25081519

Studies on chemical constituents of Gracilaria verrucosa.

PubMed

Aydoğmuş, Zeynep; Topcu, Gülaçti; Güven, Kasim Cemal

2008-12-01

A new sterol glucoside, (24R)-5 alpha-stigmast-9-(11)-en-3beta-D-glucopyranoside (1) has been isolated from a methanol extract of the red alga Gracilaria verrucosa, while cholesterol and (Z)-9-hexadecenoic acid (palmitoleic acid) have been isolated from a dichloromethane-acetone extract of the same alga. Additionally, an oily fraction of a dichloromethane-acetone extract has been investigated by gas chromatography/mass spectrometry (GC/MS). The main components in the oily fraction were heneicosanoic acid (49.8%), (Z)-9-octadecenoic acid (15.8%), and 15-tetracosenoic acid (15.6%) in addition to a few hydrocarbons, simple aromatics and a new compound, namely 3,4-dimethyl-5-carboxyclic acid-1-oxacyclopent-3-en-2-one. The structures of the isolated compounds have been elucidated by spectroscopic methods.

Evaluation, prediction and optimization the ultrasound-assisted extraction method using response surface methodology: antioxidant and biological properties of Stachys parviflora L.

PubMed

Bashi, Davoud Salar; Dowom, Samaneh Attaran; Bazzaz, Bibi Sedigheh Fazly; Khanzadeh, Farhad; Soheili, Vahid; Mohammadpour, Ali

2016-05-01

To optimize the extraction method using response surface methodology, extract the phenolic compounds, and identify the antioxidant and biological properties of Stachys parviflora L. extracts. Maceration and ultrasound-assisted extraction (UAE) (4, 7, 10 min treatment time, 40, 70, 100 % high-intensity and 60, 80, 100 % (v v-1) methanol purity) were applied to obtain the extracts. SEM was conducted to provide the microstructure of the extracted plant. MICs (colorimetric assay), MFCs (colony diameter), total phenolic content, total flavonoid content, radical scavenging capacity and extraction efficiency were determined. HPLC analysis was applied to measure the existent phenolic compounds. A quadratic model (4 min treatment time, 74.5 % high-intensity and 74.2 % solvent purity) was suggested as the best (TPC: 20.89 mg GAE g-1 d.m., TFC: 6.22 mg QEs g-1 d.m., DPPH IC50: 21.86 µg ml-1 and EE: 113.65 mg g-1 d.m.) UAE extraction model. The optimized UAE extract was generally more effective against Gram-positive microorganisms (MIC: 10-20; MBC: 10-40 (mg ml-1)) than Gram-negative ones (MIC: 40; MBC: >40 (mg ml-1)). Moreover, it (MGI: 2.32-100 %) revealed more anti-mold activity than maceration (MGI: <28.77 %). Explosive disruption of the cell walls, therefore, enhanced extraction yield by acoustic cavitation, was elucidated using SEM. Caffeic acid, tannic acid, quercetin, trans ferulic acid and rosmarinic acid were determined as the phenolic compounds in the optimized extract. RSM optimization was successfully applied for UAE from S. parviflora. The considerable antioxidant and biological properties were attributed to the phenolic compounds.

Extraction of brewer's yeasts using different methods of cell disruption for practical biodiesel production.

PubMed

Řezanka, Tomáš; Matoulková, Dagmar; Kolouchová, Irena; Masák, Jan; Viden, Ivan; Sigler, Karel

2015-05-01

The methods of preparation of fatty acids from brewer's yeast and its use in production of biofuels and in different branches of industry are described. Isolation of fatty acids from cell lipids includes cell disintegration (e.g., with liquid nitrogen, KOH, NaOH, petroleum ether, nitrogenous basic compounds, etc.) and subsequent processing of extracted lipids, including analysis of fatty acid and computing of biodiesel properties such as viscosity, density, cloud point, and cetane number. Methyl esters obtained from brewer's waste yeast are well suited for the production of biodiesel. All 49 samples (7 breweries and 7 methods) meet the requirements for biodiesel quality in both the composition of fatty acids and the properties of the biofuel required by the US and EU standards.

Phenolic Compounds and Antioxidant Activity of Phalaenopsis Orchid Hybrids

PubMed Central

Minh, Truong Ngoc; Khang, Do Tan; Tuyen, Phung Thi; Minh, Luong The; Anh, La Hoang; Quan, Nguyen Van; Ha, Pham Thi Thu; Quan, Nguyen Thanh; Toan, Nguyen Phu; Elzaawely, Abdelnaser Abdelghany; Xuan, Tran Dang

2016-01-01

Phalaenopsis spp. is the most commercially and economically important orchid, but their plant parts are often left unused, which has caused environmental problems. To date, reports on phytochemical analyses were most available on endangered and medicinal orchids. The present study was conducted to determine the total phenolics, total flavonoids, and antioxidant activity of ethanol extracts prepared from leaves and roots of six commercial hybrid Phalaenopsis spp. Leaf extracts of “Chian Xen Queen” contained the highest total phenolics with a value of 11.52 ± 0.43 mg gallic acid equivalent per g dry weight and the highest total flavonoids (4.98 ± 0.27 mg rutin equivalent per g dry weight). The antioxidant activity of root extracts evaluated by DPPH (2,2-diphenyl-1-picrylhydrazyl) free radical scavenging assay and β-carotene bleaching method was higher than those of the leaf extracts. Eleven phenolic compounds were identified, namely, protocatechuic acid, p-hydroxybenzoic acid, vanillic acid, caffeic acid, syringic acid, vanillin, ferulic acid, sinapic acid, p-coumaric acid, benzoic acid, and ellagic acid. Ferulic, p-coumaric and sinapic acids were concentrated largely in the roots. The results suggested that the root extracts from hybrid Phalaenopsis spp. could be a potential source of natural antioxidants. This study also helps to reduce the amount of this orchid waste in industrial production, as its roots can be exploited for pharmaceutical purposes. PMID:27649250

ANTI-INFLAMMATORY ACTIVITY OF EUCALYPTUS SPP. AND PISTASCIA LENTISCUS LEAF EXTRACTS

PubMed Central

Qabaha, Khaled; Ras, Sari Abu; Abbadi, Jehad; Al-Rimawi, Fuad

2016-01-01

Background: Eucalyptus spp. and Pistascia lentiscus are among the Palestinian trees that are traditionally used in folkloric medicine in treating many diseases; leaves of which are thought to have anti-inflammatory, antibacterial and antioxidant effects. The goal of this study is to evaluate the in vitro inhibitory effect of Eucalyptus spp. and Pistascia lentiscus extracts on Lipopolysacaride (LPS)-induced Interlukin-6 (Il-6) and Tumor Necrosis Factor-α (TNF-α) by polymorphonuclear Cells (PMNCs). Materials and Methods: Polymorphonuclear cells were isolated from the whole blood using Histopaque (Ficol-1077) method and then cultured in an enriched Roswell Park Memorial Institute (RBMI) medium. Supernatants’ Interlukin-6 (IL-6) and Tumor Necrosis Factor (TNF-α) levels were determined 24 hour after LPS stimulation. HPLC was employed to determine the concentration of phenolic compounds in the extracts. The concentrations of TNF-α and IL-6 were compared using paired-samples t test. Results: Eucalyptus spp. and Pistascia lentiscus leaves extracts have shown significant reduction in the levels of both Il-6 and TNF-α Gallic acid; a strong anti-inflammatory agent was found to be the major phenolic compound in both leaf extracts. However, other anti-inflammatory phenolic compounds were detected in Pitascia lentiscus extract including syringic acid and p-coumaric acid, while chlorogenic acid was detected in Eucalyptus spp. leaf extract. Conclusion: Reduction in the levels of Il-6 and TNF-α upon the effect of both Eucalyptus spp. and Pistascia lentiscus extract is an indication of their anti-inflammatory effects. Our results may also indicate that the observed anti-inflammatory effect of the above extracts may be due to the presence of gallic acid and other phenolic compounds. List of Abbreviations and Nomenclature: LPS: Lipopolysacaride, Il-6: Interlukin-6, TNF-α: Tumor Necrosis Factor-α, PMNCs: Polymorphonuclear Cells, HPLC: High Performance Liquid Chromatography, ELISA: Enzyme Linked Immune Sorbent Assay, EDTA: Ethylene Diamine Tetra Acetic acid, PBS: phosphate buffered saline, RPMI: Roswell Park Memorial Institute medium FBS: Fetal Bovine Serum. PMID:28487887

Extraction of nucleic acids from yeast cells and plant tissues using ethanol as medium for sample preservation and cell disruption.

PubMed

Linke, Bettina; Schröder, Kersten; Arter, Juliane; Gasperazzo, Tatiana; Woehlecke, Holger; Ehwald, Rudolf

2010-09-01

Here we report that dehydrated ethanol is an excellent medium for both in situ preservation of nucleic acids and cell disruption of plant and yeast cells. Cell disruption was strongly facilitated by prior dehydration of the ethanol using dehydrated zeolite. Following removal of ethanol, nucleic acids were extracted from the homogenate pellet using denaturing buffers. The method provided DNA and RNA of high yield and integrity. Whereas cell wall disruption was essential for extraction of DNA and large RNA molecules, smaller molecules such as tRNAs could be selectively extracted from undisrupted, ethanol-treated yeast cells. Our results demonstrate the utility of absolute ethanol for sample fixation, cell membrane and cell wall disruption, as well as preservation of nucleic acids during sample storage.

Fatty acid composition and preclinical resarches on Anthemis wiedemanniana Fisch. & Mey.: Discovery of a new anti-inflammatory agent

PubMed Central

Gönenç, Tuba Mert; Akkol, Esra Küpeli; Süntar, Ipek; Erdoğan, Tuğçe Fafal; Kıvçak, Bijen

2014-01-01

Background: Anthemis species have been used for the treatment of gastrointestinal disorders, hemorrhoid, stomachache and inflammatory diseases in Turkish folk medicine. Anthemis wiedemanniana Fisch. And Mey. is an endemic plant used as painkiller, antispasmodic, sedative and for the treatment of urinary inflammations. Objective: The objective of the present study is to evaluate the anti-inflamatory activity of the extracts of A. wiedemanniana by using in vivo methods. Materials and Methods: Carrageenan-, PGE2- and serotonin-induced hind paw edema, 12-O-tetradecanoyl-13-acetate (TPA)-induced mouse ear edema and acetic acid-induced increase in capillary permeability models were used for the anti-inflammatory activity assessment. Moreover, the fatty acid composition of A. wiedemanniana was investigated by gas chromatography (GC). Results: n-Hexane, diethyl ether and total sesquiterpene lactone extracts exhibited significant inhibition in carrageenan-induced hind paw edema and acetic acid-induced increase in capillary permeability model. n-Hexane and total sesquiterperne lactone extracts showed anti-inflammatory activity in PGE2- and serotonin-induced hind paw edema model. However none of the extracts displayed significant activity in TPA-induced ear edema model in mice. C4:0 (Buthyric acid), C20:0 (Arachidic acid) and C16:1 (Palmitoleik acid) were found to be the major fatty acids in these species. Saturated fatty acids (SFA) were found in higher amounts than monounsaturated fatty acids and polyunsaturated fatty acids. SFAs were determined as 63.17%, UFAs as 20.89% and PuFAs as 15.95%. Conclusion: This study confirms the traditional usage of A. wiedemanniana for inflammatory diseases. PMID:24696546

Comparison of commercial systems for extraction of nucleic acids from DNA/RNA respiratory pathogens.

PubMed

Yang, Genyan; Erdman, Dean E; Kodani, Maja; Kools, John; Bowen, Michael D; Fields, Barry S

2011-01-01

This study compared six automated nucleic acid extraction systems and one manual kit for their ability to recover nucleic acids from human nasal wash specimens spiked with five respiratory pathogens, representing Gram-positive bacteria (Streptococcus pyogenes), Gram-negative bacteria (Legionella pneumophila), DNA viruses (adenovirus), segmented RNA viruses (human influenza virus A), and non-segmented RNA viruses (respiratory syncytial virus). The robots and kit evaluated represent major commercially available methods that are capable of simultaneous extraction of DNA and RNA from respiratory specimens, and included platforms based on magnetic-bead technology (KingFisher mL, Biorobot EZ1, easyMAG, KingFisher Flex, and MagNA Pure Compact) or glass fiber filter technology (Biorobot MDX and the manual kit Allprep). All methods yielded extracts free of cross-contamination and RT-PCR inhibition. All automated systems recovered L. pneumophila and adenovirus DNA equivalently. However, the MagNA Pure protocol demonstrated more than 4-fold higher DNA recovery from the S. pyogenes than other methods. The KingFisher mL and easyMAG protocols provided 1- to 3-log wider linearity and extracted 3- to 4-fold more RNA from the human influenza virus and respiratory syncytial virus. These findings suggest that systems differed in nucleic acid recovery, reproducibility, and linearity in a pathogen specific manner. Published by Elsevier B.V.

Application of a dispersive solid-phase extraction method using an amino-based silica-coated nanomagnetic sorbent for the trace quantification of chlorophenoxyacetic acids in water samples.

PubMed

Ghambarian, Mahnaz; Behbahani, Mohammad; Esrafili, Ali; Sobhi, Hamid Reza

2017-09-01

Herein, an amino-based silica-coated nanomagnetic sorbent was applied for the effective extraction of two chlorophenoxyacetic acids (2-methyl-4-chlorophenoxyacetic acid and 2,4-dichlorophenoxyacetic acid) from various water samples. The sorbent was successfully synthesized and subsequently characterized by scanning electron microscopy, X-ray diffraction, and Fourier-transform infrared spectroscopy. The analytes were extracted by the sorbent mainly through ionic interactions. Once the extraction of analytes was completed, they were desorbed from the sorbent and detected by high-performance liquid chromatography with ultraviolet detection. A number of factors affecting the extraction and desorption of the analytes were investigated in detail and the optimum conditions were established. Under the optimum conditions, the calibration curves were linear over the concentration range of 1-250, and based on a signal-to-noise ratio of 3, the method detection limits were determined to be 0.5 μg/L for both analytes. Additionally, a preconcentration factor of 314 was achieved for the analytes. The average relative recoveries obtained from the fortified water samples varied in the range of 91-108% with relative standard deviations of 2.9-8.3%. Finally, the method was determined to be robust and effective for environmental water analysis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Simultaneous determination of phenolic acids and flavonoids in rice using solid-phase extraction and RP-HPLC with photodiode array detection.

PubMed

Irakli, Maria N; Samanidou, Victoria F; Biliaderis, Costas G; Papadoyannis, Ioannis N

2012-07-01

An analytical method based on an optimized solid-phase extraction procedure and followed by high-performance liquid chromatography (HPLC) separation with diode array detection was developed and validated for the simultaneous determination of phenolic acids (gallic, protocatechuic, 4-hydroxy-benzoic, vanillic, caffeic, syringic, p-coumaric, ferulic, sinapic, and cinnamic acids), flavanols (catechin and epicatechin), flavonols (myricetin, quercetin, kaempferol, quercetin-3-O-glucoside, hyperoside, and rutin), flavones (luteolin and apigenin) and flavanones (naringenin and hesperidin) in rice flour (Oryza sativa L.). Chromatographic separation was carried out on a PerfectSil Target ODS-3 (250 mm × 4.6 mm, 3 μm) column at temperature 25°C using a mobile phase, consisting of 0.5% (v/v) acetic acid in water, methanol, and acetonitrile at a flow rate 1 mL min(-1) , under gradient elution conditions. Application of optimum extraction conditions, elaborated on both Lichrolut C(18) and Oasis HLB cartridges, have led to extraction of phenolic acids and flavonoids from rice flour with mean recoveries 84.3-113.0%. The developed method was validated in terms of linearity, accuracy, precision, stability, and sensitivity. Repeatability (n = 5) and inter-day precision (n = 4) revealed relative standard deviation (RSD) <13%. The optimized method was successfully applied to the analysis of phenolic acids and flavonoids in pigmented (red and black rice) and non-pigmented rice (brown rice) samples. © 2012 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Determination of five arsenic species in rice by liquid chromatography-inductively coupled plasma-mass spectrometry].

PubMed

Gong, Jiadi; Cao, Xiaolin; Cao, Zhaoyun; Bian, Yingfang; Yu, Shasha; Chen, Mingxue

2014-07-01

A method was developed for the simultaneous determination of arsenic acid [As (V)], arsenious acid [As (III)], arsenobetaine (AsB), monomethylarsonic acid (MMA) and dimethylarsinic acid (DMA) in rice by liquid chromatography-inductively coupled plasma-mass spectrometry (LC-ICP-MS). The extraction reagent was 0.3 mol/L nitric acid with heat-assistant condition for 1.5 h at 95 degrees C. Then, the five arsenic species were separated by an anion exchange column (Dionex IonPac AS19, 250 mm x 4 mm) and detected by ICP-MS. Four kinds of extracted solutions were compared through the extraction efficiency. The concentration of nitric acid, the temperature and the extraction time were optimized. The recoveries of the five arsenic species spiked in rice at two levels ranged from 89.6% to 99.5% with the relative standard deviations (RSDs, n = 5) of 0.6% - 3.6%. The measured values of the arsenic species in standard rice materials were consistent with their standard values. The linear ranges were 0.05 - 200 microg/L for AsB and DMA, 0.10-400 microg/L for As (III) and MMA, 0.15-600 microg/L for As (V). The limits of detection for the five arsenic species were 0.15-0.45 microg/kg. The results showed that the method is much more precise for the risk assessment of the rice. This method is simple, accurate and durable for the determination of arsenic species in rice.

Comparison of Moringa Oleifera seeds oil characterization produced chemically and mechanically

NASA Astrophysics Data System (ADS)

Eman, N. A.; Muhamad, K. N. S.

2016-06-01

It is established that virtually every part of the Moringa oleifera tree (leaves, stem, bark, root, flowers, seeds, and seeds oil) are beneficial in some way with great benefits to human being. The tree is rich in proteins, vitamins, minerals. All Moringa oleifera food products have a very high nutritional value. They are eaten directly as food, as supplements, and as seasonings as well as fodder for animals. The purpose of this research is to investigate the effect of seeds particle size on oil extraction using chemical method (solvent extraction). Also, to compare Moringa oleifera seeds oil properties which are produced chemically (solvent extraction) and mechanically (mechanical press). The Moringa oleifera seeds were grinded, sieved, and the oil was extracted using soxhlet extraction technique with n-Hexane using three different size of sample (2mm, 1mm, and 500μm). The average oil yield was 36.1%, 40.80%, and 41.5% for 2mm, 1mm, and 500μm particle size, respectively. The properties of Moringa oleifera seeds oil were: density of 873 kg/m3, and 880 kg/m3, kinematic viscosity of 42.2mm2/s and 9.12mm2/s for the mechanical and chemical method, respectively. pH, cloud point and pour point were same for oil produced with both methods which is 6, 18°C and 12°C, respectively. For the fatty acids, the oleic acid is present with high percentage of 75.39%, and 73.60% from chemical and mechanical method, respectively. Other fatty acids are present as well in both samples which are (Gadoleic acid, Behenic acid, Palmitic acid) which are with lower percentage of 2.54%, 5.83%, and 5.73%, respectively in chemical method oil, while they present as 2.40%, 6.73%, and 6.04%, respectively in mechanical method oil. In conclusion, the results showed that both methods can produce oil with high quality. Moringa oleifera seeds oil appear to be an acceptable good source for oil rich in oleic acid which is equal to olive oil quality, that can be consumed in Malaysia where the olive oil is imported with high prices. In the same time cultivation of Moringa oleifera tree is considered to be a new source of income for the country and give more job opportunities.

Determination of volatile organic acids in oriental tobacco by needle-based derivatization headspace liquid-phase microextraction coupled to gas chromatography/mass spectrometry.

PubMed

Sun, Shi-Hao; Xie, Jian-Ping; Xie, Fu-Wei; Zong, Yong-Li

2008-02-01

A method coupling needle-based derivatization headspace liquid-phase microextraction with gas chromatography-mass spectrometry (HS-LPME/GC-MS) was developed to determine volatile organic acids in tobacco. The mixture of N,O-bis(trimethylsilyl)trifluoroacetamide and decane was utilized as the solvent for HS-LPME, resulting that extraction and derivatization were simultaneously completed in one step. The solvent served two purposes. First, it pre-concentrated volatile organic acids in the headspace of tobacco sample. Second, the volatile organic acids extracted were derivatized to form silyl derivatives in the drop. The main parameters affecting needle-based derivatization HS-LPME procedure such as extraction and derivatization reagent, microdrop volume, extraction and derivatization time, and preheating temperature and preheating time were optimized. The standard addition approach was essential to obtain accurate measurements by minimizing matrix effects. Good linearity (R(2)> or =0.9804) and good repeatability (RSDs< or =15.3%, n=5) for 16 analytes in spiked standard analytes sample were achieved. The method has the additional advantages that at the same time it is simple, fast, effective, sensitive, selective, and provides an overall profile of volatile organic acids in the oriental tobacco. This paper does offer an alternative approach to determine volatile organic acids in tobacco.

Method for the chromatographic separation of cations from aqueous samples

DOEpatents

Horwitz, E.P.; Chiarizia, R.; Dietz, M.L.

1997-07-29

An extraction chromatographic material is described for extracting metal cations from a liquid stream. The extraction chromatographic material is prepared by adsorbing a diesterified methanediphosphonic acid on an inert particulate support. 7 figs.

Phenolic acids profile, antioxidant and antibacterial activity of chamomile, common yarrow and immortelle (Asteraceae).

PubMed

Mekinić, Ivana Generalić; Skroza, Danijela; Ljubenkov, Ivica; Krstulović, Luka; Možina, Sonja Smole; Katalinić, Višnja

2014-12-01

Chamomile, common yarrow and immortelle ethanolic extracts were chemically analysed with respect to phenolics. Twelve phenolic acids were separated and identified by HPLC-DAD and the presence of rosmarinic acid was additionally confirmed by LC-MS. Five methods were applied for the evaluation of extracts' antioxidant properties (FRAP, DPPH, ABTS, chelating activity, Briggs-Rauscher reaction), while the antibacterial activity was tested against some of the major food-borne pathogens (Campylobacter coli, Escherichia coli, Salmonella Infantis, Bacillus cereus, Listeria monocytogenes and Staphylococcus aureus). Immortelle extract was the richest in phenolics with a dominant flavonoid fraction, while the other two extracts contained higher amount of non-flavonoids. The phenolic acid profile also varied; high concentration of rosmarinic acid was found in chamomile and common yarrow, while caffeic acid was dominant in immortelle. The best antioxidant properties were obtained for chamomile extract, while good antimicrobial activity, especially against Gram-positive bacterial species, was detected for immortelle. The obtained results could be used as a tool for chemotaxonomic classification of the investigated plants or for their potential application as natural antioxidants/antimicrobials.

Determination of total arsenic and arsenic(III) in phosphate fertilizers by hydride generation atomic absorption spectrometry after ultrasound-assisted extraction based on a control acid media.

PubMed

Rezende, Helen Cristine; Coelho, Nivia Maria Melo

2014-01-01

An ultrasound-assisted extraction procedure was developed for determination of inorganic arsenic (As) in phosphate fertilizer by hydride generation atomic absorption spectrometry. The variables that affect the hydride generation step were optimized, including the reducer, acid, sample flow rate, and concentrations of the acid and reducer. The determination of As(lll) was performed through the simple control of solution pH with a 0.5 M citric acid-sodium citrate buffer solution at pH 4.5, and total As was determined after a pre-reduction reaction with 1.0% (w/v) thiourea. Ultrasound-assisted acid extraction was performed, and the parameters sonication time and acid and Triton X-114 concentrations were optimized using a 23 factorial design and central composite design. LODs for As(lll) and total As were 0.029 and 0.022 microg/L, respectively. The accuracy of the method was confirmed with certified reference materials. The method was successfully applied in the determination of inorganic As in phosphate fertilizer samples.

Investigation of antioxidant ability of grape seeds extract to prevent oxidatively induced DNA damage by gas chromatography-tandem mass spectrometry.

PubMed

Aybastıer, Önder; Dawbaa, Sam; Demir, Cevdet

2018-01-01

Phenolic compounds have been studied elaborately for their efficacy to improve health and to protect against a wide variety of diseases. Herein this study, different analysis methods were implemented to evaluate the antioxidant properties of catechin and cyanidin using their standard substances and as they found in the grape seeds extracts. Total phenol contents were 107.39±8.94mg GAE/g dw of grape seeds for grape seed extract (GSE) and 218.32±10.66mg GAE/g dw of grape seeds for acid-hydrolyzed grape seed extract (AcGSE). The extracts were analyzed by HPLC-DAD system and the results showed the presence of catechin, gallic acid, chlorogenic acid and ellagic acid in the processed methanolic extract and cyanidin, gallic acid and ellagic acid in the processed acidified methanolic extract. The protective abilities of catechin and cyanidin were tested against the oxidation of DNA. The results showed that cyanidin has better protection of DNA against oxidation than catechin. GSE and AcGSE were revealed to inhibit the oxidatively induced DNA damage. GSE decreased about 57% of damage caused by the Fenton control sample. This study could show new aspects of the antioxidant profiles of cyanidin and catechin. Copyright © 2017 Elsevier B.V. All rights reserved.

Determination of haloacetic acids in water using layered double hydroxides as a sorbent in dispersive solid-phase extraction followed by liquid chromatography with tandem mass spectrometry.

PubMed

Alsharaa, Abdulnaser; Sajid, Muhammad; Basheer, Chanbasha; Alhooshani, Khalid; Lee, Hian Kee

2016-09-01

In the present study, highly efficient and simple dispersive solid-phase extraction procedure for the determination of haloacetic acids in water samples has been established. Three different types of layered double hydroxides were synthesized and used as a sorbent in dispersive solid-phase extraction. Due to the interesting behavior of layered double hydroxides in an acidic medium (pH˂4), the analyte elution step was not needed; the layered double hydroxides are simply dissolved in acid immediately after extraction to release the analytes which are then directly introduced into a liquid chromatography with tandem mass spectrometry system for analysis. Several dispersive solid-phase extraction parameters were optimized to increase the extraction efficiency of haloacetic acids such as temperature, extraction time and pH. Under optimum conditions, good linearity was achieved over the concentration range of 0.05-100 μg/L with detection limits in the range of 0.006-0.05 μg/L. The relative standard deviations were 0.33-3.64% (n = 6). The proposed method was applied to different water samples collected from a drinking water plant to determine the concentrations of haloacetic acids. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A simple and fast method based on mixed hemimicelles coated magnetite nanoparticles for simultaneous extraction of acidic and basic pollutants.

PubMed

Asgharinezhad, Ali Akbar; Ebrahimzadeh, Homeira

2016-01-01

One of the considerable and disputable areas in analytical chemistry is a single-step simultaneous extraction of acidic and basic pollutants. In this research, a simple and fast coextraction of acidic and basic pollutants (with different polarities) with the aid of magnetic dispersive micro-solid phase extraction based on mixed hemimicelles assembly was introduced for the first time. Cetyltrimethylammonium bromide (CTAB)-coated Fe3O4 nanoparticles as an efficient sorbent was successfully applied to adsorb 4-nitrophenol and 4-chlorophenol as two acidic and chlorinated aromatic amines as basic model compounds. Using a central composite design methodology combined with desirability function approach, the optimal experimental conditions were evaluated. The opted conditions were pH = 10; concentration of CTAB = 0.86 mmol L(-1); sorbent amount = 55.5 mg; sorption time = 11.0 min; no salt addition to the sample, type, and volume of the eluent = 120 μL methanol containing 5% acetic acid and 0.01 mol L(-1) HCl; and elution time = 1.0 min. Under the optimum conditions, detection limits and linear dynamic ranges were achieved in the range of 0.05-0.1 and 0.25-500 μg L(-1), respectively. The percent of extraction recoveries and relative standard deviations (n = 5) were in the range of 71.4-98.0 and 4.5-6.5, respectively. The performance of the optimized method was certified by coextraction of other acidic and basic compounds. Ultimately, the applicability of the method was successfully confirmed by the extraction and determination of the target analytes in various water samples, and satisfactory results were obtained.

Subcritical Fluid Extraction of Chinese Quince Seed: Optimization and Product Characterization.

PubMed

Wang, Li; Wu, Min; Liu, Hua-Min; Ma, Yu-Xiang; Wang, Xue-De; Qin, Guang-Yong

2017-03-25

Chinese quince seed (CQS) is an underutilized oil source and a potential source of unsaturated fatty acids and α-tocopherol-rich oil. Subcritical fluid (SCF) extraction is executed at lower pressures and temperatures than the pressures and temperatures used in supercritical fluid extraction. However, no studies on the SCF extraction of CQS oil are reported. Therefore, the objective of this study was to evaluate the use of SCF for the extraction of CQS oil and to compare the use of SCF with the classical Soxhlet (CS) and supercritical CO₂ (SC-CO₂) extraction methods. Response surface methodology (RSM) was used to investigate the extraction conditions: temperature (45-65 °C), time (30-50 min), and solvent/solid ratio (5-15 mL/g). The optimization results showed that the highest yield (27.78%) was obtained at 56.18 °C, 40.20 min, and 12.57 mL/g. The oil extracted by SCF had a higher unsaturated fatty acid content (86.37%-86.75%), higher α-tocopherol content (576.0-847.6 mg/kg), lower acid value (3.97 mg/g), and lower peroxide value (0.02 meq O₂/kg) than extractions using CS and SC-CO 2 methods. The SCF-defatted meal of oilseed exhibited the highest nitrogen solubility index (49.64%) and protein dispersibility index (50.80%), demonstrating that SCF extraction was a promising and efficient technique as an alternative to CS and SC-CO 2 methods, as very mild operating conditions and an eco-friendly solvent can be used in the process with maximum preservation of the quality of the meal.

Detection, characterization and identification of phenolic acids in Danshen using high-performance liquid chromatography with diode array detection and electrospray ionization mass spectrometry.

PubMed

Liu, Ai-Hua; Guo, Hui; Ye, Min; Lin, Yan-Hua; Sun, Jiang-Hao; Xu, Man; Guo, De-An

2007-08-17

By using HPLC-diode array detection-electrospray ion trap tandem mass spectrometry (HPLC-DAD-ESI-MS(n)) in negative ion mode, we have analyzed the fragmentation pathways of 11 phenolic acids which were isolated from Danshen. Then the extract of Danshen was analyzed, and a total of 42 phenolic acids, including sixteen new minor constituents, were identified or tentatively identified for the first time. A new solid-phase extraction (SPE) method, new HPLC separation method, new liquid chromatography (LC)-MS and LC-MS(n) (n=3-5) data and proposed fragmentation pathways, LC retention time for phenolic acids are reported.

Desulfurization of Saudi Arabian crudes by oxidation-extraction method.

PubMed

Al Otaibi, Raja L; Liu, Dong; Hou, Xulian; Song, Linhua; Li, Qingyin; Li, Mengfei; Almigrin, Hamid O; Yan, Zifeng

The oxidation-extraction desulfurization of Saudi Arabian crudes was conducted with hydrogen peroxide-acetic acid oxidation system. The selection of extractant, the optimization of oxidation-extraction conditions, and the exploration of desulfurization mechanism were studied. As DMF was used as the extractant, the optimal desulfurization rate of 35.11 % and oil recovery of 95 % were obtained at 70 °C with the molar ratio of peracetic acid to sulfur of 8:1, the molar ratio of acetic acid to hydrogen peroxide of 2:1 and the volume ratio of extractant to oil of 1:1. The desulfurization effect of different fractions in the treated Saudi Arabian crudes was found to obey the following order: gasoline-diesel fraction >VGO fraction >VR fraction, due to different types and structures of sulfur compounds. The oil quality was less affected and most sulfides were mainly extracted via DMF.

Antioxidant components of Viburnum opulus L. determined by on-line HPLC-UV-ABTS radical scavenging and LC-UV-ESI-MS methods.

PubMed

Karaçelik, Ayça Aktaş; Küçük, Murat; İskefiyeli, Zeynep; Aydemir, Sezgin; De Smet, Seppe; Miserez, Bram; Sandra, Patrick

2015-05-15

Antioxidant activity of the juice and seed and skin extracts prepared with methanol, acetonitrile, and water of Viburnum opulus L. grown in Eastern Black Sea Region were studied with an on-line HPLC-ABTS method and off-line antioxidant methods, among which a linear positive correlation was observed. The fruit extracts were analysed with the HPLC-UV method optimised with 14 standard phenolics. Identification of the phenolic components in the juice was made using an HPLC-UV-ESI-MS method. Nineteen phenolic compounds in juice were identified by comparing the retention times and mass spectra with those of the standards and the phenolics reported in the literature. The major peaks in the juice belonged to coumaroyl-quinic acid, chlorogenic acid, procyanidin B2, and procyanidin trimer. Quite different antioxidant composition profiles were obtained from the extracts with the solvents of different polarities. The antioxidant activities of the seed extracts were higher than those of the skin extracts in general. Copyright © 2014 Elsevier Ltd. All rights reserved.

Rapid ultrasonic and microwave-assisted micellar extraction of zingiberone, shogaol and gingerols from gingers using biosurfactants.

PubMed

Peng, Li-Qing; Cao, Jun; Du, Li-Jing; Zhang, Qi-Dong; Xu, Jing-Jing; Chen, Yu-Bo; Shi, Yu-Ting; Li, Rong-Rong

2017-09-15

Two kinds of extraction methods ultrasonic-assisted micellar extraction (UAME) and microwave-assisted micellar extraction (MAME) coupled with ultra-high performance liquid chromatography with ultraviolet detector (UHPLC-UV) were developed and evaluated for extraction and determination of zingerone, 6-gingerol, 8-gingerol, 6-shogaol and 10-gingerol in Rhizoma Zingiberis and Rhizoma Zingiberis Preparata. A biosurfactant, hyodeoxycholic acid sodium salt, was used in micellar extraction. Several experimental parameters were studied separately by a univariate method. The result indicated that the MAME was more efficient than UAME. The optimal conditions of MAME were as follows: 100mM of hyodeoxycholic acid sodium salt was used as surfactant, the irradiation time was set at 10s and the extraction temperature was set at 60°C. The validation results indicated that the limits of detection were in the range of 3.80-8.11ng/mL. The average recoveries were in the range of 87.32-103.12% for the two samples at two spiking levels. Compared with other reported methods, the proposed MAME-UHPLC-UV method was more effective, quicker (10s) and more eco-friendly. Copyright © 2017 Elsevier B.V. All rights reserved.

Analysis of biologically active oxyprenylated phenylpropanoids in Tea tree oil using selective solid-phase extraction with UHPLC-PDA detection.

PubMed

Scotti, Luca; Genovese, Salvatore; Bucciarelli, Tonino; Martini, Filippo; Epifano, Francesco; Fiorito, Serena; Preziuso, Francesca; Taddeo, Vito Alessandro

2018-05-30

An efficient analytical strategy based on different extraction methods of biologically active naturally occurring oxyprenylated umbelliferone and ferulic acid derivatives 7-isopentenyloxycoumarin, auraptene, umbelliprenin, boropinic acid, and 4'-geranyloxyferulic acid and quantification by UHPLC with spectrophotometric (UV/Vis) detection from Tea tree oil is reported. Absorption of the pure oil on Al 2 O 3 (Brockmann activity II) prior washing the resulting solid with MeOH and treatment of this latter with CH 2 Cl 2 resulted the best extraction methodology in terms of yields of oxyprenylated secondary metabolites. Among the five O-prenylphenylpropanoids herein under investigation auraptene and umbelliprenin were never detected while 4'-geranyloxyferulic acid was the most abundant compound resulting from all the three extraction methods employed. The UHPLC analytical methodology set up in the present study resulted to be an effective and versatile technique for the simultaneous characterization and quantification of prenyloxyphenylpropanoids in Tea tree oil and applicable to other complex matrices from the plant kingdom. Copyright © 2018 Elsevier B.V. All rights reserved.

Extraction of metals and/or metalloids from acidic media using supercritical fluids and salts

DOEpatents

Wai, Chien M.; Smart, Neil G.; Lin, Yuehe

1998-01-01

A method of extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical carbon dioxide, containing a chelating agent is described. The chelating agent forms chelates that are soluble in the fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent comprises a trialkyl phosphate, a triaryl phosphate, a trialkylphosphine oxide, a triarylphosphine oxide, or mixtures thereof. The method provides an environmentally benign process for removing contaminants from industrial waste. The method is particularly useful for extracting actinides from acidic solutions, and the process can be aided by the addition of nitrate salts. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process.

Analysis of psilocin, bufotenine and LSD in hair.

PubMed

Martin, Rafaela; Schürenkamp, Jennifer; Gasse, Angela; Pfeiffer, Heidi; Köhler, Helga

2015-03-01

A method for the simultaneous extraction of the hallucinogens psilocin, bufotenine, lysergic acid diethylamide (LSD) as well as iso-LSD, nor-LSD and O-H-LSD from hair with hydrochloride acid and methanol is presented. Clean-up of the hair extracts is performed with solid phase extraction using a mixed-mode cation exchanger. Extracts are measured with liquid chromatography coupled with electrospray tandem mass spectrometry. The method was successfully validated according to the guidelines of the 'Society of Toxicological and Forensic Chemistry' (GTFCh). To obtain reference material hair was soaked in a solution of the analytes in dimethyl sulfoxide/methanol to allow incorporation into the hair. These fortified hair samples were used for method development and can be employed as quality controls. © The Author 2014. Published by Oxford University Press. All rights reserved. For Permissions, please email: journals.permissions@oup.com.

Ethnobotanical survey, chemical composition, and antioxidant capacity of methanolic extract of the root bark of Annona cuneata Oliv.

PubMed

Khallouki, Farid; Haubner, Roswitha; Ulrich, Cornelia M; Owen, Robert W

2011-11-01

The root bark of Annona cuneata Oliv. is traditionally used in the Democratic Republic of Congo to treat several debilitating conditions, such as hernia, female sterility, sexual asthenia, and parasitic infections. However, little is known about the composition of the secondary plant substances, which may contribute to these traditional medicinal effects. We conducted an ethnobotanical study and then evaluated the composition of the secondary plant substances in extracts of the root bark by using spectroscopic methods. After delipidation, the root bark was lixiviated in methanol, and components in the extract were studied by gas chromatography-mass spectometry, high-performance liquid chromatography (HPLC)-electrospray ionization-MS and nano-electrospray ionization-MS-MS. These methods identified 13 secondary plant substances (almost exclusively phenolic compounds): p-hydroxybenzaldehyde (I), vanillin (II), tyrosol (III), 3,4-dihydroxybenzaldehyde (IV), p-hydroxybenzoic acid (V), vanillyl alcohol (VI), syringaldehyde (VII), 4-hydroxy-3-methoxyphenylethanol (VIII), vanillic acid (IX), 3,4-dihydroxybenzoic acid (X), syringic acid (XI), and ferulic acid (XII), along with the phytosterol squalene (XIII). In the HPLC-based hypoxanthine/xanthine oxidase antioxidant assay system, the methanolic extract exhibited potent antioxidant capacity, with a 50% inhibitory concentration of 72 μL, equivalent to 1.38 mg/mL of raw extract. Thus, a methanol extract of A. cuneata Oliv. contained a range of polyphenolic compounds, which may be partly responsible for its known traditional medicinal effects. More detailed studies on the phytochemistry of this important plant species are therefore warranted.

Deproteinization of water-soluble ß-glucan during acid extraction from fruiting bodies of Pleurotus ostreatus mushrooms.

PubMed

Szwengiel, Artur; Stachowiak, Barbara

2016-08-01

Some ß-glucans can be easily extracted from Basidiomycete mushrooms but commonly used extraction procedures are not satisfactory. A simultaneous method for acid extraction and deproteinization in the case of Pleurotus ostreatus was developed using response surface methodology. The optimized extraction conditions proposed here (30°C, 3.8% HCl, 300min, stirring) allow for the simultaneous extraction and deproteinization of polysaccharides. Additionally, the acid extraction yield was 7 times greater than that of hot water extraction. The combined enzymatic digestion with lyticase, ß-glucanase, exo-1,3-ß-d-glucanase, and ß-glucosidase results elucidated that an extract containing ß-1,3-ß-1,6-ß-1,4-glucan. The gel permeation chromatography (GPC) results showed that the two glucan fractions obtained do not contain linked proteins. The weight average molecular weight of the first fraction (Mw=1137kDa) was 60 times higher than that of the second fraction (Mw=19kDa). Copyright © 2016 Elsevier Ltd. All rights reserved.

Spectrophotometric determination of boric acid in boron powder with curcumin

DOE Office of Scientific and Technical Information (OSTI.GOV)

Grotheer, E.W.

1979-12-01

A rapid and accurate method was needed to determine trace amounts of boric acid for quality control and specification testing of elemental boron. The reaction between boric acid and curcumin occurs at a measurable rate only when the curcumin molecule is protonated. Protonation takes place at the carbonyl groups in the presence of a strong acid and occurs completely and rapidly when sulfuric acid is added to a solution of curcumin in acetic acid. Spectrophotometric measurements were made. The extraction of boric acid from boron powder was found to be complete within 2h when either water or the diol solutionmore » was used. Whatman No. 40 cr 42 filter paper was used to obtain diol samples free of boron particles. The extraction efficiency of 2-ethyl-1,3-hexanediol was evaluated by adding 1 ml of 500 ppM aqueous boric acid and 1 drop of 10% NaOH to accurately weighed samples of boron powder. The water then was evaporated at room temperature and the samples were extracted with diol solution. The data obtained are included. The extraction efficiency also was evaluated by determining the boric acid content of boron which had been recovered from a previous extraction and boric acid determination. The determination of boric acid using curcumin is unaffected by the presence of other compounds, except for fluoride and nitrate ions. 2 tables. (DP)« less

Selective extraction and determination of chlorogenic acids as combined quality markers in herbal medicines using molecularly imprinted polymers based on a mimic template.

PubMed

Ji, Wenhua; Zhang, Mingming; Yan, Huijiao; Zhao, Hengqiang; Mu, Yan; Guo, Lanping; Wang, Xiao

2017-12-01

We describe a solid-phase extraction adsorbent based on molecularly imprinted polymers (MIPs), prepared with use of a mimic template. The MIPs were used for the selective extraction and determination of three chlorogenic acids as combined quality markers for Lonicera japonica and Lianhua qingwen granules. The morphologies and surface groups of the MIPs were assessed by scanning electron microscopy, Brunauer-Emmett-Teller surface area analysis, and Fourier transform infrared spectroscopy. The adsorption isotherms, kinetics, and selectivity of the MIPs were systematically compared with those of non-molecularly imprinted polymers. The MIPs showed high selectivity toward three structurally similar chlorogenic acids (chlorogenic acid, cryptochlorogenic acid, and neochlorogenic acid). A procedure using molecularly imprinted solid-phase extraction coupled with high-performance liquid chromatography was established for the determination of three chlorogenic acids from Lonicera japonica and Lianhua qingwen granules. The recoveries of the chlorogenic acids ranged from 93.1% to 101.4%. The limits of detection and limits of quantification for the three chlorogenic acids were 0.003 mg g -1 and 0.01 mg g -1 , respectively. The newly developed method is thus a promising technique for the enrichment and determination of chlorogenic acids from herbal medicines. Graphical Abstract Mimic molecularly imprinted polymers for the selective extraction of chlorogenic acids.

High-throughput method based on quick, easy, cheap, effective, rugged and safe followed by liquid chromatography-multi-wavelength detection for the quantification of multiclass polyphenols in wines.

PubMed

Fontana, Ariel R; Bottini, Rubén

2014-05-16

In this work, a reliable, simple, fast, inexpensive and robust sample preparation approach for the determination of multiclass polyphenols in wine samples is proposed. The polyphenols selected for this work were gallic acid, (+)-catechin, (-)-epicatechin, caffeic acid, syringic acid, coumaric acid, ferulic acid, trans-resveratrol, quercetin and cinnamic acid. The method is based on QuEChERS (quick, easy, cheap, effective, rugged and safe) extraction technique coupled with dispersive solid-phase extraction (d-SPE) clean-up. Under optimized conditions, the analytes were extracted from 5mL wine samples (previously acidified with 1% formic acid) using 2.5mL acetonitrile. For phase separation, 1.5g NaCl and 4g anhydrous MgSO4 were added. Then, a 1mL aliquot of the partitioned supernatant was cleaned-up using d-SPE with a combination of 150mg CaCl2, 50mg primary-secondary amine (PSA) and 50mgC18 as sorbents. A 250μL aliquot of the obtained cleaned extract was concentrated to dryness and taken up with the initial mobile phase previous to liquid chromatography-multi-wavelength detection (LC-MWD). The proposed method provided limits of detection (LODs) ranging from 0.004 to 0.079μgmL(-1) and an inter-day variability below 12% RSD for all analytes in red and white wine samples. Considering external calibration (red wines) and matrix-matched calibration (white wines) as quantification techniques, the overall recoveries (accuracy) of the method ranged between 75.0% and 119.6% for red and white wine samples, respectively. The developed method was applied for the determination of polyphenols in 10 wines produced in Argentina. Nine phenolic compounds were determined, at concentrations above detectable levels in the method. The maximum concentrations corresponded to (-)-epicatechin in white wines, while gallic acid and (+)-catechin were the most abundant in red wines. Copyright © 2014 Elsevier B.V. All rights reserved.

Coupling of solvent-based de-emulsification dispersive liquid-liquid microextraction with high performance liquid chromatography for simultaneous simple and rapid trace monitoring of 2,4-dichlorophenoxyacetic acid and 2-methyl-4-chlorophenoxyacetic acid.

PubMed

Behbahani, Mohammad; Najafi, Fatemeh; Bagheri, Saman; Bojdi, Majid Kalate; Hassanlou, Parmoon Ghareh; Bagheri, Akbar

2014-04-01

A simple, rapid, and efficient sample pretreatment technique, based on solvent-based de-emulsification dispersive liquid-liquid microextraction (SD-DLLME), followed by high performance liquid chromatography (HPLC) has been developed for simultaneous preconcentration and trace detection of 2,4-dichlorophenoxyacetic acid (2,4-D) and 2-methyl-4-chlorophenoxyacetic acid (MCPA) in water and urine samples. Some parameters such as acidity of solution, the amount of salt, type, and volume of extraction solvents, type of disperser/de-emulsifier solvent, and its volume were investigated and optimized. Under optimum extraction conditions, the limits of detections (LODs) of this method for MCPA and 2,4-D were 0.2 and 0.6 μg L(-1) (based on 3S(b)/m) in water and 0.4 and 1.6 μg L(-1) in urine, respectively. Furthermore, dynamic linear range of this method for MCPA and 2,4-D was 1-300 and 2-400 μg L(-1), repectively. Finally, the applicability of the proposed method was evaluated by extraction and determination of the herbicides in urine and different water samples.

The acid tolerance response and pH adaptation of Enterococcus faecalis in extract of lime Citrus aurantiifolia from Aceh Indonesia.

PubMed

Mubarak, Zaki; Soraya, Cut

2018-01-01

Background:  The objective of the present study was to evaluate the acid tolerance response and pH adaptation when Enterococcus faecalis interacted with extract of lime ( Citrus aurant iifolia ). Methods : We used E. faecalis ATCC 29212 and lime extract from Aceh, Indonesia. The microbe was analyzed for its pH adaptation, acid tolerance response, and adhesion assay using a light microscope with a magnification of x1000. Further, statistical tests were performed to analyze both correlation and significance of the acid tolerance and pH adaptation as well as the interaction activity. Results : E. faecalis was able to adapt to a very acidic environment (pH 2.9), which was characterized by an increase in its pH (reaching 4.2) at all concentrations of the lime extract (p < 0.05). E. faecalis was also able to provide acid tolerance response to lime extract based on spectrophotometric data (595 nm) (p < 0.05). Also, the interaction activity of E. faecalis in different concentrations of lime extract was relatively stable within 6 up to 12 hours (p < 0.05), but it became unstable within 24-72 hours (p > 0.05) based on the mass profiles of its interaction activity. Conclusions : E. faecalis can adapt to acidic environments (pH 2.9-4.2); it is also able to tolerate acid generated by Citrus auranti ifolia extract, revealing a stable interaction in the first 6-12 hours.

Optimization of Protein Extraction and Two-Dimensional Electrophoresis Protocols for Oil Palm Leaf.

PubMed

Daim, Leona Daniela Jeffery; Ooi, Tony Eng Keong; Yusof, Hirzun Mohd; Majid, Nazia Abdul; Karsani, Saiful Anuar Bin

2015-08-01

Oil palm (Elaeis guineensis) is an important economic crop cultivated for its nutritional palm oil. A significant amount of effort has been undertaken to understand oil palm growth and physiology at the molecular level, particularly in genomics and transcriptomics. Recently, proteomics studies have begun to garner interest. However, this effort is impeded by technical challenges. Plant sample preparation for proteomics analysis is plagued with technical challenges due to the presence of polysaccharides, secondary metabolites and other interfering compounds. Although protein extraction methods for plant tissues exist, none work universally on all sample types. Therefore, this study aims to compare and optimize different protein extraction protocols for use with two-dimensional gel electrophoresis of young and mature leaves from the oil palm. Four protein extraction methods were evaluated: phenol-guanidine isothiocyanate, trichloroacetic acid-acetone precipitation, sucrose and trichloroacetic acid-acetone-phenol. Of these four protocols, the trichloroacetic acid-acetone-phenol method was found to give the highest resolution and most reproducible gel. The results from this study can be used in sample preparations of oil palm tissue for proteomics work.

The extraction of aromatic carboxylic acids by the copper complex with Curtis macrocyclic tetramine and its utilization for photometric determination of nonsteroidal anti-inflammatory drugs.

PubMed

Zseltvay, Ivan; Zheltvay, Olga; Antonovich, Valerij

2011-01-01

Copper complex with Curtis macrocyclic tetramine is offered as reagent for extraction-photometric determination of nonsteroidal anti-inflammatory drugs (NSAIDs), belonging to the class of aromatic carboxylic acids. The studies indicate that this method is suitable for quantitative determination of NSAIDs, which have the constant distribution in the system chloroform/water (log P) no less than 3 and dissolubility in chloroform (S) no less than 10 mg/mL. Under optimum conditions, there are liner relationships between the absorption of chloroform extracts and concentration of NSAID in the range of 0.2-4 mg/mL for indometacin (Ind), 0.2-3 mg/mL for mefenamic acid (Mef) and 0.5-3 mg/mL for diclofenac (Dic). The detection limits (S/N = 3) of Ind, Mef and Dic are 0.2, 0.1 and 0.15 mg/mL, respectively. With the help of calculating method (SPARC V4.2) it was predicted the possibility of utilization of this method for extractive-photometric determination of its detached specimen NSAID.

Characterization of gold kiwifruit pectin from fruit of different maturities and extraction methods.

PubMed

Yuliarti, Oni; Matia-Merino, Lara; Goh, Kelvin K T; Mawson, John; Williams, Martin A K; Brennan, Charles

2015-01-01

Studies on gold kiwifruit pectins are limited. In this work, the characterization of pectin isolated from two different stages of maturity of gold kiwifruit, namely early harvested fruit (EHF) and main harvested fruit (MHF) isolated by three methods (acid, water, enzymatic) was carried out. Pectins isolated from MHF were higher in galacturonic acid content (52-59% w/w) and weight-average molecular weights (Mw, 1.7-3.8 × 10(6)g/mol) compared with EHF pectins (29-49% w/w and 0.2-1.7 × 10(6)g/mol respectively). Enzymatic treatment gave the highest yield but lowest in Mw, viscosity and mechanical spectra for both maturities. The pectin of both maturities was classified as high-methoxyl pectin with the degree of esterification ranged from 82% to 90%. Water-extracted MHF pectin molecules had the highest RMS radius (182.7 nm) and Mw (3.75 × 10(6)g/mol). The water extraction method appeared to retain the native state of pectin molecules compared with acid and enzymatic extraction methods based on the Mw and viscosity data. Copyright © 2014 Elsevier Ltd. All rights reserved.

Simultaneous determination of gallic acid and gentisic acid in organic anion transporter expressing cells by liquid chromatography-tandem mass spectrometry.

PubMed

Wang, Li; Halquist, Matthew S; Sweet, Douglas H

2013-10-15

In order to elucidate the role of organic anion transporters (OATs) in the renal elimination of gallic acid and gentisic acid, a new, rapid, and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the simultaneous determination of gallic acid and gentisic acid in cell lysate, using Danshensu as the internal standard (IS). After a simple liquid-liquid extraction, the analytes were detected in negative ESI mode using selected reaction monitoring. The precursor-to-product ion transitions (m/z) were 169.0→125.0, 153.1→108.0, and 196.8→135.2 for gallic acid, gentisic acid, and the IS, respectively. Chromatographic separation was achieved on a C18 column using mobile phases consisting of water with 0.1% acetic acid (A) and acetonitrile with 0.05% formic acid. (B) The total run time was 3min and calibration curves were linear over the concentrations of 0.33-2400ng/mL for both compounds (r(2)>0.995). Good precision (between 3.11% and 14.1% RSD) and accuracy (between -12.7% and 11% bias) was observed for quality controls at concentrations of 0.33 (lower limit of quantification), 1, 50, and 2000ng/mL. The mean extraction recovery of gallic acid and gentisic acid was 80.7% and 83.5%, respectively. Results from post-column infusion and post-extraction methods indicated that the analytical method exhibited negligible matrix effects. Finally, this validated assay was successfully applied in a cellular uptake study to determine the intracellular concentrations of gallic acid and gentisic acid in OAT expressing cells. Copyright © 2013 Elsevier B.V. All rights reserved.

Pretreatment Solution for Water Recovery Systems

NASA Technical Reports Server (NTRS)

Muirhead, Dean (Inventor)

2018-01-01

Chemical pretreatments are used to produce usable water by treating a water source with a chemical pretreatment that contains a hexavalent chromium and an acid to generate a treated water source, wherein the concentration of sulfate compounds in the acid is negligible, and wherein the treated water source remains substantially free of precipitates after the addition of the chemical pretreatment. Other methods include reducing the pH in urine to be distilled for potable water extraction by pretreating the urine before distillation with a pretreatment solution comprising one or more acid sources selected from a group consisting of phosphoric acid, hydrochloric acid, and nitric acid, wherein the urine remains substantially precipitate free after the addition of the pretreatment solution. Another method described comprises a process for reducing precipitation in urine to be processed for water extraction by mixing the urine with a pretreatment solution comprising hexavalent chromium compound and phosphoric acid.

Determination of the acid value of instant noodles: interlaboratory study.

PubMed

Hakoda, Akiko; Sakaida, Kenichi; Suzuki, Tadanao; Yasui, Akemi

2006-01-01

An interlaboratory study was performed to evaluate the method for determining the acid value of instant noodles, based on the Japanese Agricultural Standard (JAS), with extraction of lipid using petroleum ether at a volume of 100 mL to the test portion of 25 g. Thirteen laboratories participated and analyzed 5 test samples as blind duplicates. Statistical treatment revealed that the repeatability (RSDr) of acid value was <6.5%, and the reproducibility (RSDR) of acid value was <9.6%. The HorRat values (RSDR/predicted RSDR) were 1.2-1.8, where the RSDR and the predicted RSDR were obtained in terms of free fatty acids in the noodles per unit weight, using the equation [acid value = percent free fatty acids (as oleic) x 1.99] and the extracted lipid contents. This method was shown to have acceptable precision by the present study.

Method for the chromatographic separation of cations from aqueous samples

DOEpatents

Horwitz, E.P.; Chiarizia, R.; Dietz, M.L.

1998-12-22

An extraction chromatographic material is described for extracting metal cations from a liquid stream. The extraction chromatographic material is prepared by adsorbing a diesterified methane-diphosphonic acid on an inert particulate support. 7 figs.

Qualitative and quantitative determination of extractives in heartwood of Scots pine (Pinus sylvestris L.) by gas chromatography.

PubMed

Ekeberg, Dag; Flaete, Per-Otto; Eikenes, Morten; Fongen, Monica; Naess-Andresen, Carl Fredrik

2006-03-24

A method for quantitative determination of extractives from heartwood of Scots pine (Pinus sylvestris L.) using gas chromatography (GC) with flame ionization detection (FID) was developed. The limit of detection (LOD) was 0.03 mg/g wood and the linear range (r = 0.9994) was up to 10 mg/g with accuracy within +/- 10% and precision of 18% relative standard deviation. The identification of the extractives was performed using gas chromatography combined with mass spectrometry (GC-MS). The yields of extraction by Soxhlet were tested for solid wood, small particles and fine powder. Small particles were chosen for further analysis. This treatment gave good yields of the most important extractives: pinosylvin, pinosylvin monomethyl ether, resin acids and free fatty acids. The method is used to demonstrate the variation of these extractives across stems and differences in north-south direction.

Fatty acids from high rate algal pond's microalgal biomass and osmotic stress effects.

PubMed

Drira, Neila; Dhouibi, Nedra; Hammami, Saoussen; Piras, Alessandra; Rosa, Antonella; Porcedda, Silvia; Dhaouadi, Hatem

2017-11-01

The extraction of oil from a wild microalgae biomass collected from a domestic wastewater treatment facility's high rate algal pond (HRAP) was investigated. An experiment plan was used to determine the most efficient extraction method, the optimal temperature, time and solvent system based on total lipids yield. Microwave-assisted extraction was the most efficient method whether in n-hexane or in a mixture of chloroform/methanol compared to Soxhlet, homogenization, and ultrasounds assisted extractions. This same wild biomass was cultivated in a photobioreactor (PBR) and the effect of osmotic stress was studied. The lipids extraction yield after 3days of stress increased by more than four folds without any significant loss of biomass, however, the quality of extracted total lipids in terms of saturated, monounsaturated and polyunsaturated fatty acids was not affected by salinity change in the culture medium. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effect of steam explosion-assisted extraction on phenolic acid profiles and antioxidant properties of wheat bran.

PubMed

Liu, Liya; Zhao, Mengli; Liu, Xingxun; Zhong, Kui; Tong, Litao; Zhou, Xianrong; Zhou, Sumei

2016-08-01

The majority of phenolic acids in wheat bran are bound to the cell walls. Hence, a high proportion of phenolic acids cannot be extracted with conventional extraction methods. This study aimed to investigate the efficiency of steam explosion pre-treatment in increasing the extractability of phenolic compounds from wheat bran. Bound phenolic acids (BPA) can be released by steam explosion-assisted extraction. Within the experimental range, soluble free phenolic acids (FPA) and soluble conjugated phenolic acids (CPA) increased gradually with residence time and temperature. After steam explosion at 215 °C for 120 s, the total FPA and CPA reached 6671.8 and 2578.6 µg GAE g(-1) bran, respectively, which was about 39-fold and seven-fold higher than that of the untreated sample. Ferulic acid, the major individual phenolic acids in bran, increased from 55.7 to 586.3 µg g(-1) for FPA, and from 44.9 to 1108.4 µg g(-1) for CPA. The antioxidant properties of FPA and CPA extracts were significantly improved after treated. Correlation analysis indicated that the antioxidant capacity was in close relationship with phenolic content in FPA and CPA. Steam explosion pre-treatment could be effectively used to release of BPA and enhance the antioxidant capacity of wheat bran. © 2015 Society of Chemical Industry. © 2015 Society of Chemical Industry.

A simple and efficient ultrasonic-assisted extraction procedure combined with UV-Vis spectrophotometry for the pre-concentration and determination of folic acid (vitamin B9) in various sample matrices.

PubMed

Gürkan, Ramazan; Altunay, Nail

2016-07-01

A simple and efficient ultrasonic-assisted extraction (UAE) procedure has been proposed for the pre-concentration of (2S)-2-[(4-{[(2-amino-4-hydroxypteridin-yl)methyl]amino}phenyl)formamido]pentanedioic acid (folic acid) in vegetables, pharmaceuticals and foods prior to determination at 540 nm using UV-Vis spectrophotometry. The method is based on hydrophobic ternary complex formation of folic acid with silver ions in the presence of cetyltrimethylammonium bromide (CTAB) as a sensitivity enhancer counter ion at pH 7.0, and then extraction into a micellar phase of polyethylene glycol monoalkyl ether (Genapol X-080). The impacts on the extraction efficiency and complex formation of analytical parameters such as sample pH, concentration of silver, concentration of surfactants and extraction time, ultrasonic time and sample volume, were investigated and optimised in detail. The matrix effect on the pre-concentration and determination of folic acid was investigated, and it was observed that the proposed method was highly selective against possible matrix co-extractives. Under optimised conditions, a good linear relationship between the analytical signal and folic acid concentration was obtained in the range of 0.6-180 μg l(-1) with a detection limit of 0.19 μg l(-1) and quantification limit of 0.63 μg l(-1). The applicability was evaluated using samples fortified at different concentration levels, and recoveries higher than 94.1% were obtained. The precision as the percent relative standard deviation (RSD%) was in range of 2.5-3.8% (10 and 40 μg l(-1), n = 5). The proposed method was validated by analysis of two standard reference materials (SRMs) and various real samples, and satisfactory results were obtained.

Hill AFB, Utah Installation Restoration Program. Phase IIB, IRP Survey. Volume 1. Text. Volume 2. Appendices

DTIC Science & Technology

1984-09-11

5 EPA 625 . Endosulfan sulfate wg/L 5 EPA 625 Chlordane pg/L * Toxaphene Pg/L * Acid Extractable Detection Analytical Compound Units Limit Method...ND ND ND ND 4,4’-DDT 5 ND ND ND ND Endosuif an sulfate 5 ND ND ND ND Chlordane* Toxa phene* Detection Acid Extractable Compound Limit M4-2 M4-6 14-9 Ge...Endosulfan sulfate 5 ND ND Chlordane * Toxaphene * Detection Acid Extractable Compound Limit BPM-1 BPM-2 2-Chlorophenol 2 ND ND 2-Nitrophenol 2 ND ND

Modified procedure to determine acid-insoluble lignin in wood and pulp

DOE Office of Scientific and Technical Information (OSTI.GOV)

Effland, M.J.

1977-10-01

If wood is treated with strong acid, carbohydrates are hydrolyzed and solubilized. The insoluble residue is by definition lignin and can be measured gravimetrically. The standard method of analysis requires samples of 1 or 2 g of wood or pulp. In research at this laboratory these amounts of sample are often not available for analytical determinations. Thus we developed a modification of the standard procedure suitable for much smaller sample amounts. The modification is based on the procedure of Saeman. Wood samples require extraction prior to lignin analysis to remove acid-insoluble extractives that will be measured as lignin. Usually thismore » involves only a standard extraction with ethanol--benzene. However, woods high in tannin must also be subjected to extraction with alcohol. Pulps seldom require extraction.« less

Extracts of Phenolic Compounds from Seeds of Three Wild Grapevines—Comparison of Their Antioxidant Activities and the Content of Phenolic Compounds

PubMed Central

Weidner, Stanisław; Powałka, Anna; Karamać, Magdalena; Amarowicz, Ryszard

2012-01-01

Phenolic compounds were extracted from three wild grapevine species: Vitis californica, V. riparia and V. amurensis seeds using 80% methanol or 80% acetone. The total content of phenolic compounds was determined utilizing the Folin-Ciocalteu’s phenol reagent while the content of tannins was assayed with the vanillin and BSA precipitation methods. Additionally, the DPPH free radical scavenging activity and the reduction power of the extracts were measured. The RP-HPLC method was applied to identify the phenolic compounds in the extracts, such as phenolic acids and catechins. The seeds contained large amounts of tannins, catechins and gallic acid and observable quantities of p-coumaric acid. The total content of phenolic compounds and tannins was similar in the extracts from V. californica and V. riparia seeds. However, the total content of total phenolic compounds and tannins in the extracts from V. californica and V. riperia seeds were about two-fold higher than that in the extracts from V. amurensis seeds. Extracts from seeds of the American species (V. californica and V. riparia) contained similarly high concentrations of tannins, whereas extracts from seeds of V. amurensis had approximately half that amount of these compounds. The content of catechin and epicatechin was similar in all extracts. The highest DPPH• anti-radical scavenging activity was observed in the acetonic and methanolic extracts of V. californica and V. riparia seeds— while the acetonic extract from the V. californica seeds was the strongest reducing agent. PMID:22489161

Comparative pharmacokinetics of chlorogenic acid after oral administration in rats

PubMed Central

Qi, Wei; Zhao, Ting; Yang, Wen-Wen; Wang, Guang-Hou; Yu, Hua; Zhao, Hai-Xiao; Yang, Chen; Sun, Li-Xin

2011-01-01

The present study was aimed at the comparison of the pharmacokinetics of pure chlorogenic acid and extract of Solanum lyratum Thunb. The animals were allocated to two groups, and were administered chlorogenic acid or extract of S. lyratum Thunb. at a dose of 50.0 mg/kg orally. Blood samples were collected up to 8 h post-dosing. Plasma chlorogenic acid analyses were performed using an HPLC method with UV detector. The pharmacokinetic parameters were evaluated using non-compartmental assessment. Significant differences existed in the two groups for AUC0−t, AUC0−∞ and CLz/F. The reliable HPLC method was successfully applied to the determination of chlorogenic acid in rat plasma at dosage of 50.0 mg/kg. PMID:29403709

Optimisation of Microwave-Assisted Extraction of Pomegranate (Punica granatum L.) Seed Oil and Evaluation 
of Its Physicochemical and Bioactive Properties

PubMed Central

Çavdar, Hasene Keskin; Gök, Uğur; Göğüş, Fahrettin

2017-01-01

Summary Pomegranate seed oil was extracted in a closed-vessel high-pressure microwave system. The characteristics of the obtained oil, such as fatty acid composition, free fatty acidity, total phenolic content, antioxidant activity and colour, were compared to those of the oil obtained by cold solvent extraction. Response surface methodology was applied to optimise extraction conditions: power (176–300 W), time (5–20 min), particle size (d=0.125–0.800 mm) and solvent to sample ratio (2:1, 6:1 and 10:1, by mass). The predicted highest extraction yield (35.19%) was obtained using microwave power of 220 W, particle size in the range of d=0.125–0.450 mm and solvent-to-sample ratio of 10:1 (by mass) in 5 min extraction time. Microwave-assisted solvent extraction (MASE) resulted in higher extraction yield than that of Soxhlet (34.70% in 8 h) or cold (17.50% in 8 h) extraction. The dominant fatty acid of pomegranate seed oil was punicic acid (86%) irrespective of the extraction method. Oil obtained by MASE had better physicochemical properties, total phenolic content and antioxidant activity than the oil obtained by cold solvent extraction. PMID:28559737

Quantitation of phosphatidic acid and lysophosphatidic acid molecular species using hydrophilic interaction liquid chromatography coupled to electrospray ionization high resolution mass spectrometry.

PubMed

Triebl, Alexander; Trötzmüller, Martin; Eberl, Anita; Hanel, Pia; Hartler, Jürgen; Köfeler, Harald C

2014-06-20

A method for a highly selective and sensitive identification and quantitation of lysophosphatidic acid (LPA) and phosphatidic acid (PA) molecular species was developed using hydrophilic interaction liquid chromatography (HILIC) followed by negative-ion electrospray ionization high resolution mass spectrometry. Different extraction methods for the polar LPA and PA species were compared and a modified Bligh & Dyer extraction by addition of 0.1M hydrochloric acid resulted in a ≈1.2-fold increase of recovery for the 7 PA and a more than 15-fold increase for the 6 LPA molecular species of a commercially available natural mix compared to conventional Bligh & Dyer extraction. This modified Bligh & Dyer extraction did not show any artifacts resulting from hydrolysis of natural abundant phospholipids. The developed HILIC method is able to separate all PA and LPA species from major polar membrane lipid classes which might have suppressive effects on the minor abundant lipid classes of interest. The elemental compositions of intact lipid species are provided by the high mass resolution of 100,000 and high mass accuracy below 3ppm of the Orbitrap instrument. Additionally, tandem mass spectra were generated in a parallel data dependent acquisition mode in the linear ion trap to provide structural information at molecular level. Limits of quantitation were identified at 45fmol on column and the dynamic range reaches 20pmol on column, covering the range of natural abundance well. By applying the developed method to mouse brain it can be shown that phosphatidic acid contains less unsaturated fatty acids with PA 34:1 and PA 36:1 as the major species. In contrast, for LPA species a high content of polyunsaturated fatty acids (LPA 20:4 and LPA 22:6) was quantified. Copyright © 2014 Elsevier B.V. All rights reserved.

Comparison of hot hydroxylamine hydrochloride and oxalic acid leaching of stream sediment and coated rock samples as anomaly enhancement techniques

USGS Publications Warehouse

Filipek, L.H.; Chao, T.T.; Theobald, P.K.

1982-01-01

A hot hydroxylamine hydrochloride (H-Hxl) extraction in 25% acetic acid is compared with the commonly used oxalic acid extraction as a method of anomaly enhancement for Cu and Zn in samples from two very different metal deposits and climatic environments. Results obtained on minus-80-mesh stream sediments from an area near the Magruder massive sulfide deposit in Lincoln County, Georgia, where the climate is humid subtropical, indicate that H-Hxl enhances the anomaly for Cu by a factor of 2 and for Zn by a factor of 1.5, compared to the oxalic method. Analyses of Fe oxide-coated rock samples from outcrops overlying the North Silver Bell porphyry copper deposit near Tucson, Arizona, where the climate is semi-arid to arid, indicate that both techniques effectively outline the zones of hydrothermal alteration. The H-Hxl extraction can also perform well in high-carbonate or high-clay environments, where other workers have suggested that oxalic acid is not very effective. Therefore, the H-Hxl method is recommended for general exploration use. ?? 1982.

Simultaneous Analysis of Ursolic Acid and Oleanolic Acid in Guava Leaves Using QuEChERS-Based Extraction Followed by High-Performance Liquid Chromatography

PubMed Central

Xu, Chang; Liao, Yiyi; Fang, Chunyan; Zhang, Yingxia

2017-01-01

In this paper, a novel method of QuEChERS-based extraction coupled with high-performance liquid chromatography has been developed for the simultaneous determination of ursolic acid (UA) and oleanolic acid (OA) in guava leaves. The QuEChERS-based extraction parameters, including the amount of added salt, vortex-assisted extraction time, and absorbent amount, and the chromatographic conditions were investigated for the analysis of UA and OA in guava leaves. Under the optimized conditions, the method showed good linearity over a range of 1–320 μg mL−1, with correlation coefficients above 0.999. The limits of detection of UA and OA were 0.18 and 0.36 μg mL−1, respectively. The intraday and interday precision were below 1.95 and 2.55%, respectively. The accuracies of the UA and OA determinations ranged from 97.4 to 111.4%. The contents of UA and OA in the guava leaf samples were 2.50 and 0.73 mg g−1, respectively. These results demonstrate that the developed method is applicable to the simultaneous determination of UA and OA in guava leaves. PMID:28781908

Direct quantification of fatty acids in wet microalgal and yeast biomass via a rapid in situ fatty acid methyl ester derivatization approach.

PubMed

Dong, Tao; Yu, Liang; Gao, Difeng; Yu, Xiaochen; Miao, Chao; Zheng, Yubin; Lian, Jieni; Li, Tingting; Chen, Shulin

2015-12-01

Accurate determination of fatty acid contents is routinely required in microalgal and yeast biofuel studies. A method of rapid in situ fatty acid methyl ester (FAME) derivatization directly from wet fresh microalgal and yeast biomass was developed in this study. This method does not require prior solvent extraction or dehydration. FAMEs were prepared with a sequential alkaline hydrolysis (15 min at 85 °C) and acidic esterification (15 min at 85 °C) process. The resulting FAMEs were extracted into n-hexane and analyzed using gas chromatography. The effects of each processing parameter (temperature, reaction time, and water content) upon the lipids quantification in the alkaline hydrolysis step were evaluated with a full factorial design. This method could tolerate water content up to 20% (v/v) in total reaction volume, which equaled up to 1.2 mL of water in biomass slurry (with 0.05-25 mg of fatty acid). There were no significant differences in FAME quantification (p>0.05) between the standard AOAC 991.39 method and the proposed wet in situ FAME preparation method. This fatty acid quantification method is applicable to fresh wet biomass of a wide range of microalgae and yeast species.

Simultaneous Determination of Crypto-Chlorogenic Acid, Isoquercetin, and Astragalin Contents in Moringa oleifera Leaf Extracts by TLC-Densitometric Method.

PubMed

Vongsak, Boonyadist; Sithisarn, Pongtip; Gritsanapan, Wandee

2013-01-01

Moringa oleifera Lamarck (Moringaceae) is used as a multipurpose medicinal plant for the treatment of various diseases. Isoquercetin, astragalin, and crypto-chlorogenic acid have been previously found to be major active components in the leaves of this plant. In this study, a thin-layer-chromatography (TLC-)densitometric method was developed and validated for simultaneous quantification of these major components in the 70% ethanolic extracts of M. oleifera leaves collected from 12 locations. The average amounts of crypto-chlorogenic acid, isoquercetin, and astragalin were found to be 0.0473, 0.0427, and 0.0534% dry weight, respectively. The method was validated for linearity, precision, accuracy, limit of detection, limit of quantitation, and robustness. The linearity was obtained in the range of 100-500 ng/spot with a correlation coefficient (r) over 0.9961. Intraday and interday precisions demonstrated relative standard deviations of less than 5%. The accuracy of the method was confirmed by determining the recovery. The average recoveries of each component from the extracts were in the range of 98.28 to 99.65%. Additionally, the leaves from Chiang Mai province contained the highest amounts of all active components. The proposed TLC-densitometric method was simple, accurate, precise, and cost-effective for routine quality controlling of M. oleifera leaf extracts.

A green analytical chemistry approach for lipid extraction: computation methods in the selection of green solvents as alternative to hexane.

PubMed

Cascant, Mari Merce; Breil, Cassandra; Garrigues, Salvador; de la Guardia, Miguel; Fabiano-Tixier, Anne Silvie; Chemat, Farid

2017-05-01

There is a great interest in finding alternatives and green solvents in extraction processes to replace petroleum based solvents. In order to investigate these possibilities, computational methods, as Hansen solubility parameters (HSP) and conductor-like screening model for real solvent (COSMO-RS), were used in this work to predict the solvation power of a series of solvents in salmon fish lipids. Additionally, experimental studies were used to evaluate the performance in lipids extraction using 2-methyltetrahydrofurane, cyclopentyl methyl ether, dimethyl carbonate, isopropanol, ethanol, ethyl acetate, p-cymene and d-limonene compared with hexane. Lipid classes of extracts were obtained by using high performance thin-layer chromatography (HPTLC), whereas gas chromatography with a flame ionization detector (GC/FID) technique was employed to obtain fatty acid profiles. Some differences between theoretical and experimental results were observed, especially regarding the behavior of p-cymene and d-limonene, which separate from the predicted capability. Results obtained from HPTLC indicated that p-cymene and d-limonene extract triglycerides (TAGs) and diglycerides (DAGs) at levels of 73 and 19%, respectively, whereas the other studied extracts contain between 75 and 76% of TAGs and between 16 and 17% of DAGs. Fatty acid profiles, obtained by using GC-FID, indicated that saturated fatty acids (SFAs) between 19.5 and 19.9% of extracted oil, monounsaturated fatty acids (MUFAs) in the range between 43.5 and 44.9%, and PUFAs between 31.2 and 34.6% were extracted. p-Cymene and limonene extracts contained lower percentages than the other studied solvents of some PUFAs due probably to the fact that these unsaturated fatty acids are more susceptible to oxidative degradation than MUFAs. Ethyl acetate has been found to be the best alternative solvent to hexane for the extraction of salmon oil lipids. Graphical Abstract ᅟ.

Optimized Extraction Method To Remove Humic Acid Interferences from Soil Samples Prior to Microbial Proteome Measurements

DOE Office of Scientific and Technical Information (OSTI.GOV)

Qian, Chen; Hettich, Robert L.

The microbial composition and their activities in soil environments play a critical role in organic matter transformation and nutrient cycling, perhaps most specifically with respect to impact on plant growth but also more broadly to global impact on carbon and nitrogen-cycling. Liquid chromatography coupled to high performance mass spectrometry provides a powerful approach to characterize soil microbiomes; however, the limited microbial biomass and the presence of abundant interferences in soil samples present major challenges to soil proteome extraction and subsequent MS measurement. To address some of the major issues, we have designed and optimized an experimental method to enhance microbialmore » proteome extraction concomitant with minimizing the soil-borne humic substances co-extraction from soils. Among the range of interferences, humic substances are often the worst in terms of adversely impacting proteome extraction and mass spectrometry measurement. Our approach employs an in-situ detergent-based microbial lysis / TCA precipitation coupled with an additional acidification precipitation step at the peptide level which efficiently removes humic acids. By combing filtration and pH adjustment of the final peptide solution, the remaining humic acids can be differentially precipitated and removed with a membrane filter, thereby leaving much cleaner proteolytic peptide samples for MS measurement. As a result, this modified method is a reliable and straight-forward protein extraction method that efficiently removes soil-borne humic substances without inducing proteome sample loss or reducing or biasing protein identification in mass spectrometry.« less

Optimized Extraction Method To Remove Humic Acid Interferences from Soil Samples Prior to Microbial Proteome Measurements

DOE PAGES

Qian, Chen; Hettich, Robert L.

2017-05-24

The microbial composition and their activities in soil environments play a critical role in organic matter transformation and nutrient cycling, perhaps most specifically with respect to impact on plant growth but also more broadly to global impact on carbon and nitrogen-cycling. Liquid chromatography coupled to high performance mass spectrometry provides a powerful approach to characterize soil microbiomes; however, the limited microbial biomass and the presence of abundant interferences in soil samples present major challenges to soil proteome extraction and subsequent MS measurement. To address some of the major issues, we have designed and optimized an experimental method to enhance microbialmore » proteome extraction concomitant with minimizing the soil-borne humic substances co-extraction from soils. Among the range of interferences, humic substances are often the worst in terms of adversely impacting proteome extraction and mass spectrometry measurement. Our approach employs an in-situ detergent-based microbial lysis / TCA precipitation coupled with an additional acidification precipitation step at the peptide level which efficiently removes humic acids. By combing filtration and pH adjustment of the final peptide solution, the remaining humic acids can be differentially precipitated and removed with a membrane filter, thereby leaving much cleaner proteolytic peptide samples for MS measurement. As a result, this modified method is a reliable and straight-forward protein extraction method that efficiently removes soil-borne humic substances without inducing proteome sample loss or reducing or biasing protein identification in mass spectrometry.« less

Comparative Evaluation of Polyphenol Contents and Antioxidant Activities between Ethanol Extracts of Vitex negundo and Vitex trifolia L. Leaves by Different Methods.

PubMed

Saklani, Sarla; Mishra, Abhay Prakash; Chandra, Harish; Atanassova, Maria Stefanova; Stankovic, Milan; Sati, Bhawana; Shariati, Mohammad Ali; Nigam, Manisha; Khan, Mohammad Usman; Plygun, Sergey; Elmsellem, Hicham; Suleria, Hafiz Ansar Rasul

2017-09-27

The in vitro antioxidant potential assay between ethanolic extracts of two species from the genus Vitex ( Vitex negundo L. and Vitex trifolia L.) belonging to the Lamiaceae family were evaluated. The antioxidant properties of different extracts prepared from both plant species were evaluated by different methods. DPPH scavenging, nitric oxide scavenging, and β-carotene-linoleic acid and ferrous ion chelation methods were applied. The antioxidant activities of these two species were compared to standard antioxidants such as butylated hydroxytoluene (BHT), ascorbic acid, and Ethylene diamine tetra acetic acid (EDTA). Both species of Vitex showed significant antioxidant activity in all of the tested methods. As compared to V. trifolia L. (60.87-89.99%; 40.0-226.7 μg/mL), V. negundo has been found to hold higher antioxidant activity (62.6-94.22%; IC 50 = 23.5-208.3 μg/mL) in all assays. In accordance with antioxidant activity, total polyphenol contents in V. negundo possessed greater phenolic (89.71 mg GAE/g dry weight of extract) and flavonoid content (63.11 mg QE/g dry weight of extract) as compared to that of V. trifolia (77.20 mg GAE/g and 57.41 mg QE/g dry weight of extract respectively). Our study revealed the significant correlation between the antioxidant activity and total phenolic and flavonoid contents of both plant species.

Preconcentration and Determination of Mefenamic Acid in Pharmaceutical and Biological Fluid Samples by Polymer-grafted Silica Gel Solid-phase Extraction Following High Performance Liquid Chromatography

PubMed Central

Bagheri Sadeghi, Hayedeh; Panahi, Homayon Ahmad; Mahabadi, Mahsa; Moniri, Elham

2015-01-01

Mefenamic acid is a nonsteroidal anti-inflammatory drug (NSAID) that has analgesic, anti-infammatory and antipyretic actions. It is used to relieve mild to moderate pains. Solid-phase extraction of mefenamic acid by a polymer grafted to silica gel is reported. Poly allyl glycidyl ether/iminodiacetic acid-co-N, N-dimethylacrylamide was synthesized and grafted to silica gel and was used as an adsorbent for extraction of trace mefenamic acid in pharmaceutical and biological samples. Different factors affecting the extraction method were investigated and optimum conditions were obtained. The optimum pH value for sorption of mefenamic acid was 4.0. The sorption capacity of grafted adsorbent was 7.0 mg/g. The best eluent solvent was found to be trifluoroacetic acid-acetic acid in methanol with a recovery of 99.6%. The equilibrium adsorption data of mefenamic acid by grafted silica gel was analyzed by Langmuir model. The conformation of obtained data to Langmuir isotherm model reveals the homogeneous binding sites of grafted silica gel surface. Kinetic study of the mefenamic acid sorption by grafted silica gel indicates the good accessibility of the active sites in the grafted polymer. The sorption rate of the investigated mefenamic acid on the grafted silica gel was less than 5 min. This novel synthesized adsorbent can be successfully applied for the extraction of trace mefenamic acid in human plasma, urine and pharmaceutical samples. PMID:26330865

Determination of arsenic species in solid matrices utilizing supercritical fluid extraction coupled with gas chromatography after derivatization with thioglycolic acid n-butyl ester.

PubMed

Wang, Zhifeng; Cui, Zhaojie

2016-12-01

A method using derivatization and supercritical fluid extraction coupled with gas chromatography was developed for the analysis of dimethylarsinate, monomethylarsonate and inorganic arsenic simultaneously in solid matrices. Thioglycolic acid n-butyl ester was used as a novel derivatizing reagent. A systematic discussion was made to investigate the effects of pressure, temperature, flow rate of the supercritical CO 2 , extraction time, concentration of the modifier, and microemulsion on extraction efficiency. The application for real environmental samples was also studied. Results showed that thioglycolic acid n-butyl ester was an effective derivatizing reagent that could be applied for arsenic speciation. Using methanol as modifier of the supercritical CO 2 can raise the extraction efficiency, which can be further enhanced by adding a microemulsion that contains Triton X-405. The optimum extraction conditions were: 25 MPa, 90°C, static extraction for 10 min, dynamic extraction for 25 min with a flow rate of 2.0 mL/min of supercritical CO 2 modified by 5% v/v methanol and microemulsion. The detection limits of dimethylarsinate, monomethylarsonate, and inorganic arsenic in solid matrices were 0.12, 0.26, and 1.1 mg/kg, respectively. The optimized method was sensitive, convenient, and reliable for the extraction and analysis of different arsenic species in solid samples. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Analysis of Polyphenolic Compounds in Extracts from Leaves of Some Malus domestica Cultivars: Antiradical and Antimicrobial Analysis of These Extracts

PubMed Central

Sowa, Alina; Zgórka, Grażyna; Szykuła, Aleksandra; Franiczek, Roman; Żbikowska, Beata; Gamian, Andrzej

2016-01-01

In this study, methanol, ethyl acetate, water extracts, and precipitate were obtained from leaves of Malus domestica cultivars: Golden delicious, Jonagold, Elstar, Ligol, and Mutsu. Antiradical activity of these extracts was measured using the ABTS+∙ radical, and antimicrobial activity was measured with the disk-diffusion method. Phenolic compounds were measured with the colorimetric method and identified with high performance liquid chromatography (HPLC). The highest antiradical activity was observed for the Jonagold variety, and in particular strong activity was noted for ethyl acetate extracts. Antimicrobial activity was observed against strains of Staphylococcus aureus, Enterococcus faecalis, and the fungus Candida glabrata. Particularly susceptible to the extracts activity appeared to be Staphylococcus aureus, but the growth of Candida glabrata was inhibited in the presence of ethyl acetate extracts. With the HPLC method we identified a high amount of phloridzin (above 500 mg per g of ethyl acetate extracts), lower amounts of hyperoside, isoquercitrin, and quercitrin, and traces of p-hydroxybenzoic and chlorogenic acids. The contribution of phloridzin to antiradical activity of methanol and ethyl acetate extracts was very high (above 90%). In water extract the contribution of phloridzin was between 38.9 and 55.2%, chlorogenic acid 22.7 and 36.1%, and hyperoside 12.2 and 13.3%. PMID:28097143

Analysis of Polyphenolic Compounds in Extracts from Leaves of Some Malus domestica Cultivars: Antiradical and Antimicrobial Analysis of These Extracts.

PubMed

Sowa, Alina; Zgórka, Grażyna; Szykuła, Aleksandra; Franiczek, Roman; Żbikowska, Beata; Gamian, Andrzej; Sroka, Zbigniew

2016-01-01

In this study, methanol, ethyl acetate, water extracts, and precipitate were obtained from leaves of Malus domestica cultivars: Golden delicious, Jonagold, Elstar, Ligol, and Mutsu. Antiradical activity of these extracts was measured using the ABTS +∙ radical, and antimicrobial activity was measured with the disk-diffusion method. Phenolic compounds were measured with the colorimetric method and identified with high performance liquid chromatography (HPLC). The highest antiradical activity was observed for the Jonagold variety, and in particular strong activity was noted for ethyl acetate extracts. Antimicrobial activity was observed against strains of Staphylococcus aureus , Enterococcus faecalis , and the fungus Candida glabrata . Particularly susceptible to the extracts activity appeared to be Staphylococcus aureus , but the growth of Candida glabrata was inhibited in the presence of ethyl acetate extracts. With the HPLC method we identified a high amount of phloridzin (above 500 mg per g of ethyl acetate extracts), lower amounts of hyperoside, isoquercitrin, and quercitrin, and traces of p -hydroxybenzoic and chlorogenic acids. The contribution of phloridzin to antiradical activity of methanol and ethyl acetate extracts was very high (above 90%). In water extract the contribution of phloridzin was between 38.9 and 55.2%, chlorogenic acid 22.7 and 36.1%, and hyperoside 12.2 and 13.3%.

Evaluation of the antibacterial activity of the methylene chloride extract of Miconia ligustroides, isolated triterpene acids, and ursolic acid derivatives.

PubMed

Cunha, Wilson R; de Matos, Geilton X; Souza, Maria Goreti M; Tozatti, Marcos G; Andrade e Silva, Márcio L; Martins, Carlos H G; da Silva, Rosangela; Da Silva Filho, Ademar A

2010-02-01

The methylene chloride extract of Miconia ligustroides (DC.) Naudin (Melastomataceae), the isolated compounds ursolic and oleanolic acids and a mixture of these acids, and ursolic acid derivatives were evaluated against the following microorganisms: Bacillus cereus (ATCC 14579), Vibrio cholerae (ATCC 9458), Salmonella choleraesuis (ATCC 10708), Klebsiella pneumoniae (ATCC 10031), and Streptococcus pneumoniae (ATCC 6305). The microdilution method was used for determination of the minimum inhibitory concentration (MIC) during evaluation of the antibacterial activity. The methylene chloride extract showed no activity against the selected microorganisms. Ursolic acid was active against B. cereus, showing a MIC value of 20 microg/mL. Oleanolic acid was effective against B. cereus and S. pneumoniae with a MIC of 80 microg/mL in both cases. The mixture of triterpenes, ursolic and oleanolic acids, did not enhance the antimicrobial activity. However, the acetyl and methyl ester derivatives, prepared from ursolic acid, increased the inhibitory activity for S. pneumoniae.

Improved method for extracting lanthanides and actinides from acid solutions

DOEpatents

Horwitz, E.P.; Kalina, D.G.; Kaplan, L.; Mason, G.W.

1983-07-26

A process for the recovery of actinide and lanthanide values from aqueous acidic solutions uses a new series of neutral bi-functional extractants, the alkyl(phenyl)-N,N-dialkylcarbamoylmethylphosphine oxides. The process is suitable for the separation of actinide and lanthanide values from fission product values found together in high-level nuclear reprocessing waste solutions.

A new ultra-high pressure liquid chromatography method for the determination of antioxidant flavonol aglycones in six Lysimachia species.

PubMed

Tóth, Anita; Végh, Krisztina; Alberti, Ágnes; Béni, Szabolcs; Kéry, Ágnes

2016-10-01

UPLC-DAD method was developed and validated for the quantitative determination of free flavonol aglycones (kaempferol, quercetin and myricetin) after acidic hydrolysis in six Lysimachia species. Quantitative analyses showed that the amounts of various flavonol aglycones were significantly different in Lysimachia vulgaris, Lysimachia nummularia, Lysimachia punctata, Lysimachia christinae, Lysimachia ciliata and Lysimachia clethroides. The L. clethroides sample was found to be the richest in kaempferol (25.77 ± 1.29 μg/mg extract) and quercetin (97.67 ± 4.61 μg/mg extract), while the L. nummularia sample contained the highest amount of myricetin (20.79 ± 1.00 μg/mg extract). The antioxidant capacity of hydrolysed extracts was evaluated using in vitro DPPH(•) (2,2-diphenyl-1-picrylhydrazyl) and ABTS(•+) [2,2'-azino-bis-(3-ethylbenzothiazoline-6-sulphonic acid)] decolourisation tests. The observed radical scavenging capacities of the extracts showed a relationship with the measured flavonol aglycone content and composition. The acidic treatment resulted in an increased free radical scavenging activity compared to the untreated methanol extract.

[Preparation and applications of a supported liquid-liquid extraction column with a composite diatomite material].

PubMed

Bao, Jianmin; Ma, Zhishuang; Sun, Ying; Wang, Yongzun; Li, Youxin

2012-08-01

A rapid and special supported liquid-liquid extraction (SLE) column was developed with a composite diatomite material. The SLE column was evaluated by high performance liquid chromatography (HPLC) with acidic, neutral and alkaline compounds dissolved in water. Furthermore, some real complex samples were also analyzed by HPLC with the SLE method. The recoveries of benzoic acid (acidic), p-nitroaniline (alkaline) and 4-hydroxy-benzoic methyl ester (neutral) treated by the SLE column were 90.6%, 98.1% and 97.7%. However, the recoveries of the three compounds treated by traditional liquid-liquid extraction (LLE) method were 71.9%, 81.9% and 83.9%. The results showed that the SLE technique had higher recoveries than the traditional LLE method. The spiked recoveries of the complex samples, such as benzoic acid in Sprite and dexamethasone acetate, chlorphenamine maleate, indomethacin in bovine serum, were between 80% and 110% and the relative standard deviations (RSDs) were less than 15%. For biological specimen, the results could be accepted. Meantime, many disadvantages associated with traditional LLE method, such as emulsion formation, didn't occur using SLE column. The SLE column technique is a good sample preparation method with many advantages, such as rapid, simple, robust, easily automated, high recovery and high-throughput, which would be widely used in the future.

A novel fatty-acid-based in-tube dispersive liquid-liquid microextraction technique for the rapid determination of nonylphenol and 4-tert-octylphenol in aqueous samples using high-performance liquid chromatography-ultraviolet detection.

PubMed

Shih, Hou-Kuang; Shu, Ting-Yun; Ponnusamy, Vinoth Kumar; Jen, Jen-Fon

2015-01-07

In this study, a novel fatty-acid-based in-tube dispersive liquid-liquid microextraction (FA-IT-DLLME) technique is proposed for the first time and is developed as a simple, rapid and eco-friendly sample extraction method for the determination of alkylphenols in aqueous samples using high-performance liquid chromatography-ultraviolet detection (HPLC-UV). In this extraction method, medium-chain saturated fatty acids were investigated as a pH-dependent phase because they acted as either anionic surfactants or neutral extraction solvents based on the acid-base reaction caused solely by the adjustment of the pH of the solution. A specially designed home-made glass extraction tube with a built-in scaled capillary tube was utilized as the phase-separation device for the FA-IT-DLLME to collect and measure the separated extractant phase for analysis. Nonylphenol (NP) and 4-tert-octylphenol (4-tOP) were chosen as model analytes. The parameters influencing the FA-IT-DLLME were thoroughly investigated and optimized. Under the optimal conditions, the detector responses of NP and 4-tOP were linear in the concentration ranges of 5-4000 μg L(-1), with correlation coefficients of 0.9990 and 0.9996 for NP and 4-tOP, respectively. The limits of detection based on a signal-to-noise ratio of 3 were 0.7 and 0.5 μg L(-1), and the enrichment factors were 195 and 143 for NP and 4-tOP, respectively. The applicability of the developed method was demonstrated for the analysis of alkylphenols in environmental wastewater samples, and the recoveries ranged from 92.9 to 107.1%. The extraction process required less than 4 min and utilized only acids, alkalis, and fatty acids to achieve the extraction. The results demonstrated that the presented FA-IT-DLLME approach is highly cost-effective, simple, rapid and environmentally friendly in its sample preparation. Copyright © 2014 Elsevier B.V. All rights reserved.

Isolation of quercetin and mandelic acid from Aesculus indica fruit and their biological activities.

PubMed

Zahoor, Muhammad; Shafiq, Sadaf; Ullah, Habib; Sadiq, Abdul; Ullah, Farhat

2018-06-26

In this study Aesculus indica fruit was subjected to isolation of phytochemicals. Two antioxidants quercetin and Mandelic acid were isolated in pure state. The free radical scavenging and acetyl choline esterase inhibitory potential of the crude extract and sub fractions were also determined. The antioxidant capacity of crude extract, fractions and isolated compounds were determined by DPPH and ABTS methods. Folin-Ciocalteu reagent method was used to estimate the total phenolic contents and were found to be 78.34 ± 0.96, 44.16 ± 1.05, 65.45 ± 1.29, 37.85 ± 1.44 and 50.23 ± 2.431 (mg/g of gallic acid) in crude extract, ethyl acetate, chloroform, n-hexane and aqueous fractions respectively. The flavonoid concentration in crude extract, ethyl acetate, chloroform, n-hexane and aqueous fraction were; 85.30 ± 1.20, 53.80 ± 1.07, 77.50 ± 1.12, 26.30 ± 1.35 and 37.78 ± 1.25 (mg/g of quercetin) respectively. The chloroform fraction was more potent against enzymes, acetyl choline esterase and butyryl choline esterase (IC 50  = 85 and 160 μg/ml respectively). The phenolic compounds in the crude extract and fractions were determined using HPLC standard method. Chlorogenic acid, quercetin, phloroglucinol, rutin, mandelic acid and hydroxy benzoic acid were detected at retention times 6.005, 10.062, 22.623, 30.597, 35.490 and 36.211 in crude extract and different fractions. The ethyl acetate fraction was rich in the targeted compounds and was therefore subjected to column isolation. The HPLC chromatogram of isolated compounds showed single peak at specified retention times which confirms their isolation in pure state. The isolated compounds were then characterized by FTIR and NMR spectrophotometric techniques. The Aesculus indica fruit extracts showed antioxidant and anticholine esterase inhibitory potentials. Two bioactive compounds were isolated in the pure form ethyl acetate fraction. From results it was concluded that the fruit of this plant could be used to minimize oxidative stress caused by reactive oxygen species.

In vitro evaluation of antioxidant activity of Cordia dichotoma (Forst f.) bark

PubMed Central

Nariya, Pankaj B.; Bhalodia, Nayan R.; Shukla, Vinay J.; Acharya, Rabinarayan; Nariya, Mukesh B.

2013-01-01

Cordia dichotoma Forst. f. bark, identified as botanical source of Shleshmataka in Ayurvedic pharmacopoeia. Present investigation was undertaken to evaluate possible antioxidant potential of methanolic and butanol extract of C. dichotoma bark. In vitro antioxidant activity of methanolic and butanol extract was determined by 1,1, diphenyl–2, picrylhydrazyl (DPPH) free radical scavenging assay. The extracts were also evaluated for their phenolic contents and antioxidant activity. Phenolic content was measured using Folin–Ciocalteu reagent and was calculated as Gallic acid equivalents. Antiradical activity of methanolic extract was measured by DPPH assay and was compared to ascorbic acid and ferric reducing power of the extract was evaluated by Oyaizu method. In the present study three in vitro models were used to evaluate antioxidant activity. The first two methods were for direct measurement of radical scavenging activity and remaining one method evaluated the reducing power. The present study revealed that the C. dichotoma bark has significant radical scavenging activity. PMID:24049418

In vitro evaluation of antioxidant activity of Cordia dichotoma (Forst f.) bark.

PubMed

Nariya, Pankaj B; Bhalodia, Nayan R; Shukla, Vinay J; Acharya, Rabinarayan; Nariya, Mukesh B

2013-01-01

Cordia dichotoma Forst. f. bark, identified as botanical source of Shleshmataka in Ayurvedic pharmacopoeia. Present investigation was undertaken to evaluate possible antioxidant potential of methanolic and butanol extract of C. dichotoma bark. In vitro antioxidant activity of methanolic and butanol extract was determined by 1,1, diphenyl-2, picrylhydrazyl (DPPH) free radical scavenging assay. The extracts were also evaluated for their phenolic contents and antioxidant activity. Phenolic content was measured using Folin-Ciocalteu reagent and was calculated as Gallic acid equivalents. Antiradical activity of methanolic extract was measured by DPPH assay and was compared to ascorbic acid and ferric reducing power of the extract was evaluated by Oyaizu method. In the present study three in vitro models were used to evaluate antioxidant activity. The first two methods were for direct measurement of radical scavenging activity and remaining one method evaluated the reducing power. The present study revealed that the C. dichotoma bark has significant radical scavenging activity.

Simultaneous analysis of retinol, all-trans- and 13-cis-retinoic acid and 13-cis-4-oxoretinoic acid in plasma by liquid chromatography using on-column concentration after single-phase fluid extraction.

PubMed

Teerlink, T; Copper, M P; Klaassen, I; Braakhuis, B J

1997-06-20

A reversed-phase high-performance liquid chromatographic method for the simultaneous analysis of retinol, all-trans-retinoic acid, 13-cis-retinoic acid and 13-cis-4-oxoretinoic acid in human plasma and cell culture medium is described. Sample preparation involves precipitation of proteins and extraction of retinoids with 60% acetonitrile. After centrifugation, the acetonitrile content of the supernatant is reduced to 45%, allowing on-column concentration of analytes. Injection volumes up to 2.0 ml (equivalent to 0.525 ml of sample) can be used without compromising chromatographic resolution of all-trans-retinoic acid and 13-cis-retinoic acid. Retinoids were stable in this extract and showed no isomerization when stored in the dark in a cooled autosampler, allowing automated analysis of large series of samples. Recoveries from spiked plasma samples were between 95 and 103%. Although no internal standard was used, the inter-assay precision for all retinoids was better than 6% and 4% at concentrations of 30 nM and 100 nM, respectively. The method is a valuable tool for the study of cellular metabolism of all-trans-retinoic acid, as polar metabolites of this compound can be detected with high sensitivity in cell culture media.

Extraction and Chromatographic Determination of Shikimic Acid in Chinese Conifer Needles with 1-Benzyl-3-methylimidazolium Bromide Ionic Liquid Aqueous Solutions

PubMed Central

Chen, Fengli; Hou, Kexin; Li, Shuangyang; Zu, Yuangang; Yang, Lei

2014-01-01

An ionic liquids-based ultrasound-assisted extraction (ILUAE) method was successfully developed for extracting shikimic acid from conifer needles. Eleven 1-alkyl-3-methylimidazolium ionic liquids with different cations and anions were investigated and 1-benzyl-3-methylimidazolium bromide solution was selected as the solvent. The conditions for ILUAE, including the ionic liquid concentration, ultrasound power, ultrasound time, and liquid-solid ratio, were optimized. The proposed method had good recovery (99.37%–100.11%) and reproducibility (RSD, n = 6; 3.6%). ILUAE was an efficient, rapid, and simple sample preparation technique that showed high reproducibility. Based on the results, a number of plant species, namely, Picea koraiensis, Picea meyeri, Pinus elliottii, and Pinus banksiana, were identified as among the best resources of shikimic acid. PMID:24782942

Extraction of metals and/or metalloids from acidic media using supercritical fluids and salts

DOEpatents

Wai, C.M.; Smart, N.G.; Lin, Y.

1998-06-23

A method is described for extracting metalloid and metal species from a solid or liquid material by exposing the material to a fluid solvent, particularly supercritical carbon dioxide, containing a chelating agent. The chelating agent forms chelates that are soluble in the fluid to allow removal of the species from the material. In preferred embodiments, the extraction solvent is supercritical carbon dioxide and the chelating agent comprises a trialkyl phosphate, a triaryl phosphate, a trialkylphosphine oxide, a triarylphosphine oxide, or mixtures thereof. The method provides an environmentally benign process for removing contaminants from industrial waste. The method is particularly useful for extracting actinides from acidic solutions, and the process can be aided by the addition of nitrate salts. The chelate and supercritical fluid can be regenerated, and the contaminant species recovered, to provide an economic, efficient process. 7 figs.

Detection of lysergic acid diethylamide (LSD) in urine by gas chromatography-ion trap tandem mass spectrometry.

PubMed

Sklerov, J H; Kalasinsky, K S; Ehorn, C A

1999-10-01

A confirmatory method for the detection and quantitation of lysergic acid diethylamide (LSD) is presented. The method employs gas chromatography-tandem mass spectrometry (GC-MS-MS) using an internal ionization ion trap detector for sensitive MS-MS-in-time measurements of LSD extracted from urine. Following a single-step solid-phase extraction of 5 mL of urine, underivatized LSD can be measured with limits of quantitation and detection of 80 and 20 pg/mL, respectively. Temperature-programmed on-column injections of urine extracts were linear over the concentration range 20-2000 pg/mL (r2 = 0.999). Intraday and interday coefficients of variation were < 6% and < 13%, respectively. This procedure has been applied to quality-control specimens and LSD-positive samples in this laboratory. Comparisons with alternate GC-MS methods and extraction procedures are discussed.

Evaluation of different extraction methods from pomegranate whole fruit or peels and the antioxidant and antiproliferative activity of the polyphenolic fraction.

PubMed

Masci, Alessandra; Coccia, Andrea; Lendaro, Eugenio; Mosca, Luciana; Paolicelli, Patrizia; Cesa, Stefania

2016-07-01

Pomegranate is a functional food of great interest, due to its multiple beneficial effects on human health. This fruit is rich in anthocyanins and ellagitannins, which exert a protective role towards degenerative diseases. The aim of the present work was to optimize the extraction procedure, from different parts of the fruit, to obtain extracts enriched in selected polyphenols while retaining biological activity. Whole fruits or peels of pomegranate cultivars, with different geographic origin, were subjected to several extraction methods. The obtained extracts were analyzed for polyphenolic content, evaluated for antioxidant capacity and tested for antiproliferative activity on human bladder cancer T24 cells. Two different extraction procedures, employing ethyl acetate as a solvent, were useful in obtaining extracts enriched in ellagic acid and/or punicalagins. Antioxidative and antiproliferative assays demonstrated that the antioxidant capability is directly related to the phenolic content, whereas the antiproliferative activity is to be mainly attributed to ellagic acid. Copyright © 2016 Elsevier Ltd. All rights reserved.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harman-Ware, Anne E.; Sykes, Robert; Peter, Gary F.

Terpenoids, naturally occurring compounds derived from isoprene units present in pine oleoresin, are a valuable source of chemicals used in solvents, fragrances, flavors, and have shown potential use as a biofuel. This paper describes a method to extract and analyze the terpenoids present in loblolly pine saplings and pine lighter wood. Various extraction solvents were tested over different times and temperatures. Samples were analyzed by pyrolysis-molecular beam mass spectrometry before and after extractions to monitor the extraction efficiency. The pyrolysis studies indicated that the optimal extraction method used a 1:1 hexane/acetone solvent system at 22°C for 1 h. Extracts frommore » the hexane/acetone experiments were analyzed using a low thermal mass modular accelerated column heater for fast-GC/FID analysis. The most abundant terpenoids from the pine samples were quantified, using standard curves, and included the monoterpenes, α- and β-pinene, camphene, and δ-carene. Sesquiterpenes analyzed included caryophyllene, humulene, and α-bisabolene. In conclusion, diterpenoid resin acids were quantified in derivatized extractions, including pimaric, isopimaric, levopimaric, palustric, dehydroabietic, abietic, and neoabietic acids.« less

Optimization of total vaporization solid-phase microextraction (TV-SPME) for the determination of lipid profiles of Phormia regina, a forensically important blow fly species.

PubMed

Kranz, William; Carroll, Clinton; Dixon, Darren; Picard, Christine; Goodpaster, John

2017-11-01

A new method has been developed for the determination of fatty acids, sterols, and other lipids which naturally occur within pupae of the blow fly Phormia regina. The method relies upon liquid extraction in non-polar solvent, followed by derivatization using N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) w/ 1% trimethylchlorsilane (TMCS) carried out inside the sample vial. The analysis is facilitated by total vaporization solid-phase microextraction (TV-SPME), with gas chromatography-mass spectrometry (GC-MS) serving as the instrumentation for analysis. The TV-SPME delivery technique is approximately a factor of five more sensitive than traditional liquid injection, which may alleviate the need for rotary evaporation, reconstitution, collection of high performance liquid chromatography fractions, and many of the other pre-concentration steps that are commonplace in the current literature. Furthermore, the ability to derivatize the liquid extract in a single easy step while increasing sensitivity represents an improvement over current derivatization methods. The most common lipids identified in fly pupae were various saturated and unsaturated fatty acids ranging from lauric acid (12:0) to arachinoic acid (20:4), as well as cholesterol. The concentrations of myristic acid (14:0), palmitelaidic acid (16:2), and palmitoleic acid (16:1) were the most reliable indicators of the age of the pupae. Graphical abstract Blow fly pupae were extracted prior to emerging as adults. The extracts were analyzed via total vaporization solid-phase microextraction (TV-SPME), revealing a complex mixture of lipids that could be associated with the age of the insect. This information may assist in determining a post-mortum interval (PMI) in a death investigation.

UHPLC/HR-ESI-MS/MS Profiling of Phenolics from Tunisian Lycium arabicum Boiss. Antioxidant and Anti-lipase Activities' Evaluation.

PubMed

Affes, Marwa; Fakhfakh, Jawhar; Daoud, Ines; Brieudes, Vincent; Halabalaki, Maria; El Feki, Abdelfattah; Allouche, Noureddine

2017-09-01

This study was performed in the aim to evaluate nine different extracts from Tunisian Lycium arabicum for their total phenolic and total flavonoid contents, phytochemical analyses as well as their antioxidant and anti-lipase activities. The in vitro antioxidant property was investigated using three complementary methods (DPPH, ferric reducing antioxidant power (FRAP), and β-carotene-linoleic acid bleaching assays) while anti-lipase activity was evaluated using 4-methylumbelliferyl oleate method. From all of the tested extracts the most potent found to be the polar MeOH extracts especially those of stems and leaves. In order to investigate the chemical composition of these extracts and possible correlation of their constituents with the observed activities, an UHPLC/HR-ESI-MS/MS analysis was performed. Several compounds belonging to different chemical classes were tentatively identified such as rutin and kampferol rutinoside, the major constituents of the leaves, and N-caffeoyltyramine, lyciumide A, N-dihydrocaffeoyltyramine as well as fatty acids: trihydroxyoctadecadienoic acid and hydroxyoctadecadienoic acid isomers were detected abundantly in the stems. These results showed that the MeOH extracts of stems and leaves of L. arabicum can be considered as a potential source of biological active compounds. © 2017 Wiley-VHCA AG, Zurich, Switzerland.

Study on the extraction, purification and quantification of jasmonic acid, abscisic acid and indole-3-acetic acid in plants.

PubMed

Zhang, Feng Juan; Jin, You Ju; Xu, Xing You; Lu, Rong Chun; Chen, Hua Jun

2008-01-01

Jasmonic acid (JA), abscisic acid (ABA) and indole-3-acetic acid (IAA) are important plant hormones. Plant hormones are difficult to analyse because they occur in small concentrations and other substances in the plant interfere with their detection. To develop a new, inexpensive procedure for the rapid extraction and purification of IAA, ABA and JA from various plant species. Samples were prepared by extraction of plant tissues with methanol and ethyl acetate. Then the extracts were further purified and enriched with C(18) cartridges. The final extracts were derivatised with diazomethane and then measured by GC-MS. The results of the new methodology were compared with those of the Creelman and Mullet procedure. Sequential elution of the assimilates from the C(18 )cartridges revealed that IAA and ABA eluted in 40% methanol, while JA subsequently eluted in 60% methanol. The new plant hormone extraction and purification procedure produced results that were comparable to those obtained with the Creelman and Mullet's procedure. This new procedure requires only 0.5 g leaf samples to quantify these compounds with high reliability and can simultaneously determine the concentrations of the three plant hormones. A simple, inexpensive method was developed for determining endogenous IAA, ABA and JA concentrations in plant tissue.

Nucleic acid extraction techniques and application to the microchip.

PubMed

Price, Carol W; Leslie, Daniel C; Landers, James P

2009-09-07

As recently as the early 1990s, DNA purification was time-consuming, requiring the use of toxic, hazardous reagents. The advent of solid phase extraction techniques and the availability of commercial kits for quick and reliable DNA extraction has relegated those early techniques largely to the history books. High quality DNA can now be extracted from whole blood, serum, saliva, urine, stool, cerebral spinal fluid, tissues, and cells in less time without sacrificing recovery. Having achieved such a radical change in the methodology of DNA extraction, focus has shifted to adapting these methods to a miniaturized system, or "lab-on-a-chip" (A. Manz, N. Graber and H. M. Widmer, Sens. Actuators, B, 1990, 1, 244-248). Manz et al.'s concept of a "miniaturized total chemical analysis system" (microTAS) involved a silicon chip that incorporated sample pretreatment, separation and detection. This review will focus on the first of these steps, sample pretreatment in the form of DNA purification. The intention of this review is to provide an overview of the fundamentals of nucleic acid purification and solid phase extraction (SPE) and to discuss specific microchip DNA extraction successes and challenges. In order to fully appreciate the advances in DNA purification, a brief review of the history of DNA extraction is provided so that the reader has an understanding of the impact that the development of SPE techniques have had. This review will highlight the different methods of nucleic acid extraction (Table 1), including relevant citations, but without an exhaustive summary of the literature. A recent review by Wen et al. (J. Wen, L. A. Legendre, J. M. Bienvenue and J. P. Landers, Anal. Chem., 2008, 80, 6472-6479) covers solid phase extraction methods with a greater focus on their incorporation into integrated microfluidic systems.

Examination of soil contaminated by coal-liquids by size exclusion chromatography in 1-methyl-2-pyrrolidinone solution to evaluate interference from humic and fulvic acids and extracts from peat.

PubMed

Morgan, T J; Herod, A A; Brain, S A; Chambers, F M; Kandiyoti, R

2005-11-18

Soil from a redundant coke oven site has been examined by extraction of soluble materials using 1-methyl-2-pyrrolidinone (NMP) followed by size exclusion chromatography (SEC) of the extracted material. The extracted material was found to closely resemble a high temperature coal tar pitch. Standard humic and fulvic acids were also examined since these materials are very soluble in NMP and would be extracted with pitch if present in the soil. Humic substances derived from peat samples and NMP-extracts of peats were also examined. The results show that the humic and fulvic substances were not extracted directly by NMP from peats. They were extracted using caustic soda solution and were different from the peat extracts in NMP. These results indicate that humic and fulvic acids were soluble in NMP in the protonated polyelectrolyte form but not in the original native polyelectrolyte form. The extraction of soil using NMP followed by SEC appears to be a promising method for identifying contamination by coal-based industries.

Preparation of [13C3]-melamine and [13C3]-cyanuric acid and their application to the analysis of melamine and cyanuric acid in meat and pet food using liquid chromatography-tandem mass spectrometry.

PubMed

Varelis, P; Jeskelis, R

2008-10-01

For the determination of melamine and cyanuric acid the labelled internal standards [(13)C(3)]-melamine and [(13)C(3)]-cyanuric acid were synthesized using the common substrate [(13)C(3)]-cyanuric chloride by reaction with ammonia and acidified water, respectively. Standards with excellent isotopic and chemical purities were obtained in acceptable yields. These compounds were used to develop an isotope dilution liquid chromatography/mass spectrometry (LC/MS) method to determine melamine and cyanuric acid in catfish, pork, chicken, and pet food. The method involved extraction into aqueous methanol, liquid-liquid extraction and ion exchange solid phase clean-up, with normal phase high-performance liquid chromatography (HPLC) in the so-called hydrophilic interaction mode. The method had a limit of detection (LOD) of 10 microg kg(-1) for both melamine and cyanuric acid in the four foods with a percentage coefficient of variation (CV) of less than 10%. The recovery of the method at this level was in the range of 87-110% and 96-110% for melamine and cyanuric acid, respectively.

Chemical composition and biological properties of Satureja avromanica Maroofi.

PubMed

Abdali, Elham; Javadi, Shima; Akhgari, Maryam; Hosseini, Seyran; Dastan, Dara

2017-03-01

Satureja avromanica is an indigenous plant which is frequently used as a spice in Avraman-Kurdistan region of Iran. The present study aimed to investigate the chemical composition, antimicrobial and antioxidant properties of the S. avromanica . In addition, rosmarinic acid and total phenolic content of S. avromanica was assessed by spectrophotometric method and HPTLC. The essential oil and methanolic extract were isolated by hydrodistillation and maceration methods, respectively. A total of 32 compounds representing 98.6% of the essential oil were identified by GC-MS and GC-FID. The main constituents were n -pentacosane (23.8%), spathulenol (11.5%), β-bourbonen (11.3%) and n -docosane (11.0%). The antibacterial activity of samples were carried out by disc diffusion method and evaluate the minimal inhibitory concentration (MIC) essential oil and methanolic extract were found to be effective against Staphylococcus aureus , Bacillus cereus and Bacillus pumilus . The highest scavenging activity was found for methanolic extract of S. avromanica (21.58 µg/mL) and the total phenolics of methanolic extract of S. avromanica was 95.3 mg GAE/g. The rosmarinic acid content of S. avromanica methanolic extract was 0.83 mg/g plant. Antioxidant activity and rosmarininc acid content of S. avromanica suggests that the essential oil and methanolic extract of S. avromanica has great potential for application as a natural antimicrobial and antioxidant agent to preserve food.

Necessity of purification during bacterial DNA extraction with environmental soils

PubMed Central

Choi, Jung-Hyun

2017-01-01

Complexity and heterogeneity of soil samples have often implied the inclusion of purification steps in conventional DNA extraction for polymerase chain reaction (PCR) assays. Unfortunately the purification steps are also time and labor intensive. Therefore the necessity of DNA purification was re-visited and investigated for a variety of environmental soil samples that contained various amounts of PCR inhibitors. Bead beating and centrifugation was used as the baseline (without purification) method for DNA extraction. Its performance was compared with that of conventional DNA extraction kit (with purification). The necessity criteria for DNA purification were established with environmental soil samples. Using lysis conditions at 3000 rpm for 3 minutes with 0.1 mm glass beads, centrifugation time of 10 minutes and 1:10 dilution ratio, the baseline method outperformed conventional DNA extraction on cell seeded sand samples. Further investigation with PCR inhibitors (i.e., humic acids, clay, and magnesium [Mg]) showed that sand samples containing less than 10 μg/g humic acids and 70% clay may not require purifications. Interestingly, the inhibition pattern of Mg ion was different from other inhibitors due to the complexation interaction of Mg ion with DNA fragments. It was concluded that DNA extraction method without purification is suitable for soil samples that have less than 10 μg/g of humic acids, less than 70% clay content and less than 0.01% Mg ion content. PMID:28793754

Ultrasound-assisted Extraction of Ursolic Acid from the Flowers of Ixora coccinia Linn (Rubiaceae) and Antiproliferative Activity of Ursolic Acid and Synthesized Derivatives

PubMed Central

Alves Monteath, Silvana Amadeu Ferreira; Maciel, Maria Aparecida M.; Vega, Raquel Garcia; de Mello, Heloisa; de Araújo Martins, Carollina; Esteves-Souza, Andressa; Gattass, Cerli Rocha; Echevarria, Aurea

2017-01-01

Background: Ixora coccinea Linn (Rubiaceae) is an evergreen shrub with bright scarlet colored flowers found in several tropical and subtropical countries. It is used as an ornamental and medicinal plant. Phytochemical studies revealed that its major special metabolites are triterpene acids, such as ursolic and oleanolic acid. Objective: To evaluate the isolation of ursolic acid (UA) (1) from methanol extracts of I. coccinea flowers through two methodologies, to prepare four derivatives, and to evaluate the cytotoxic effect against six cancer cell lines. Materials and Methods: The UA was isolated from vegetal material by percolation at room temperature and by ultrasound-assisted extraction. The preparation of derivatives was performed according to literature methods, and the cytotoxic effects were evaluated using the MTT (3,4,5-dimethylthiazol-2-yl-2,5-diphenyltetrazolium bromide) assay. Results: The most efficient extraction was achieved through ultrasound irradiation with a yield of 35% after KOH-impregnated silica in chromatography column. Furthermore, four derivatives (3, 5, 6, 7) of UA were prepared and evaluated, including 1, against two lung cancer (A549 and H460) and four leukemia (K562, Lucena, HL60, and Jurkat) cell lines. Generally, results showed that 1 and 7 were the most active compounds against the assayed cell lines. Also, the cytotoxic effects observed on terpenes 1 and 7 were higher when compared with cisplatin, used as positive control, with the exception of Jurkat cell line. Conclusion: The efficiency of such an alternative extraction method led to the principal and abundant active component, 1, of I. coccinea, thus representing a considerable contribution for promising triterpenoid in cancer chemotherapy. SUMMARY The ultrasound-assisted extraction of Ixora coccinea flowers improved of the ursolic acid isolationMethanolic extract from flowers of I. coccinea provided, by ultrasound irradiation, after KOH-impregnated silica in chromatography column, the ursolic acid in 35% yieldThe ursolic acid and four derivatives were prepared and assayed against two lung cancer and four leukaemia cell linesThe ursolic acid and their 3-oxo-derivative, in general, were more cytotoxic when compared to cisplatin, used as positive control Abbreviations used: MTT: 3,4,5-dimethylthiazol-2-yl-2,5-diphenyltetrazolium bromide, RP: reverse phase, TLC: thin layer chromatography, KOH: potassium hydroxide, IR: infrared, DMF: dimethylformamide, DMSO: dimethyl sulfoxide, TEA: triethylamine, RT: room temperature, EtOAc: ethyl acetate, MeOH: methanol, i-PrOH: iso-propanol, NMR: nuclear magnetic resonance, MDR: multiple drug resistance, RPMI: Roswell Park Memorial Institute PMID:28539719

Subcritical water extraction of lipids from wet algal biomass

DOEpatents

Deng, Shuguang; Reddy, Harvind K.; Schaub, Tanner; Holguin, Francisco Omar

2016-05-03

Methods of lipid extraction from biomass, in particular wet algae, through conventionally heated subcritical water, and microwave-assisted subcritical water. In one embodiment, fatty acid methyl esters from solids in a polar phase are further extracted to increase biofuel production.

Development and application of UHPLC-MS/MS method for the determination of phenolic compounds in Chamomile flowers and Chamomile tea extracts.

PubMed

Nováková, Lucie; Vildová, Anna; Mateus, Joana Patricia; Gonçalves, Tiago; Solich, Petr

2010-09-15

UHPLC-MS/MS method using BEH C18 analytical column was developed for the separation and quantitation of 12 phenolic compounds of Chamomile (Matricaria recutita L.). The separation was accomplished using gradient elution with mobile phase consisting of methanol and formic acid 0.1%. ESI in both positive and negative ion mode was optimized with the aim to reach high sensitivity and selectivity for quantitation using SRM experiment. ESI in negative ion mode was found to be more convenient for quantitative analysis of all phenolics except of chlorogenic acid and kaempherol, which demonstrated better results of linearity, accuracy and precision in ESI positive ion mode. The results of method validation confirmed, that developed UHPLC-MS/MS method was convenient and reliable for the determination of phenolic compounds in Chamomile extracts with linearity >0.9982, accuracy within 76.7-126.7% and precision within 2.2-12.7% at three spiked concentration levels. Method sensitivity expressed as LOQ was typically 5-20 nmol/l. Extracts of Chamomile flowers and Chamomile tea were subjected to UHPLC-MS/MS analysis. The most abundant phenolic compounds in both Chamomile flowers and Chamomile tea extracts were chlorogenic acid, umbelliferone, apigenin and apigenin-7-glucoside. In Chamomile tea extracts there was greater abundance of flavonoid glycosides such as rutin or quercitrin, while the aglycone apigenin and its glycoside were present in lower amount. Copyright (c) 2010 Elsevier B.V. All rights reserved.

Lipids and Fatty Acids in Algae: Extraction, Fractionation into Lipid Classes, and Analysis by Gas Chromatography Coupled with Flame Ionization Detector (GC-FID).

PubMed

Guihéneuf, Freddy; Schmid, Matthias; Stengel, Dagmar B

2015-01-01

Despite the number of biochemical studies exploring algal lipids and fatty acid biosynthesis pathways and profiles, analytical methods used by phycologists for this purpose are often diverse and incompletely described. Potential confusion and potential variability of the results between studies can therefore occur due to change of protocols for lipid extraction and fractionation, as well as fatty acid methyl esters (FAME) preparation before gas chromatography (GC) analyses. Here, we describe a step-by-step procedure for the profiling of neutral and polar lipids using techniques such as solid-liquid extraction (SLE), thin-layer chromatography (TLC), and gas chromatography coupled with flame ionization detector (GC-FID). As an example, in this protocol chapter, analyses of neutral and polar lipids from the marine microalga Pavlova lutheri (an EPA/DHA-rich haptophyte) will be outlined to describe the distribution of fatty acid residues within its major lipid classes. This method has been proven to be a reliable technique to assess changes in lipid and fatty acid profiles in several other microalgal species and seaweeds.

Method for extracting lanthanides and actinides from acid solutions by modification of purex solvent

DOEpatents

Horwitz, E. Philip; Kalina, Dale G.

1986-01-01

A process for the recovery of actinide and lanthanide values from aqueous solutions with an extraction solution containing an organic extractant having the formula: ##STR1## where .phi. is phenyl, R.sup.1 is a straight or branched alkyl or alkoxyalkyl containing from 6 to 12 carbon atoms and R.sup.2 is an alkyl containing from 3 to 6 carbon atoms and phase modifiers in a water-immiscible hydrocarbon diluent. The addition of the extractant to the Purex process extractant, tri-n-butylphosphate in normal paraffin hydrocarbon diluent, will permit the extraction of multivalent lanthanide and actinide values from 0.1 to 12.0 molar acid solutions.

A hollow-fiber membrane extraction process for recovery and separation of lactic acid from aqueous solution.

PubMed

Huang, Hanjing; Yang, Shang-Tian; Ramey, David E

2004-01-01

An energy-efficient hollow-fiber membrane extraction process was successfully developed to separate and recover lactic acid produced in fermentation. Although many fermentation processes have been developed for lactic acid production, an economical method for lactic acid recovery from the fermentation broth is still needed. Continuous extraction of lactic acid from a simulated aqueous stream was achieved by using Alamine 336 in 2-octanol contained in a hollow-fiber membrane extractor. In this process, the extractant was simultaneously regenerated by stripping with NaOH in a second membrane extractor, and the final product is a concentrated lactate salt solution. The extraction rate increased linearly with an increase in the Alamine 336 content in the solvent (from 5 to 40%). Increasing the concentration of the undissociated lactic acid in the feed solution by either increasing the lactate concentration (from 5 to 40 g/L) or decreasing the solution pH (from 5.0 to 4.0) also increased the extraction rate. Based on these observations, a reactive extraction model with a first-order reaction mechanism for both lactic acid and amine concentrations was proposed. The extraction rate also increased with an increase in the feed flow rate, but not the flow rates of solvent and the stripping solution, suggesting that the process was not limited by diffusion in the liquid films or membrane pores. A mathematical model considering both diffusion and chemical reaction in the extractor and back extractor was developed to simulate the process. The model fits the experimental data well and can be used in scale up design of the process.

Removal of interfering nucleotides from brain extracts containing substance p. Effect of drugs on brain concentrations of substance p

PubMed Central

Laszlo, I.

1963-01-01

Several methods for removing interfering nucleotides, adenosine-5'-monophosphate and adenosine 5'-triphosphate from brain extracts have been studied. An enzymic method, using adenylic acid deaminase, has been found suitable. This deaminates adenosine monophosphate to 5'-inosinic acid, an inactive compound which does not influence the estimations of substance P. Owing to the adenosine triphosphatase content of the enzyme extract, adenosine triphosphate was also inactivated. For the estimation of adenosine monophosphate-deaminase activity, a simple colorimetric method is described which measures the ammonia liberated from adenosine monophosphate. Substance P in mouse brain extracts was estimated after treatment of the animals with various drugs, and after the enzymic removal of interfering nucleotides from the brain extracts. The drugs had no effect on the substance P content of mouse brain. The effect of drugs on the contractions of the guinea-pig ileum induced by substance P was also investigated, and the effect of drugs on the estimations of substance P in brain extracts is discussed. PMID:14066136

Variability of protein content in calcium oxalate monohydrate stones.

PubMed

Williams, James C; Zarse, Chad A; Jackson, Molly E; Witzmann, Frank A; McAteer, James A

2006-08-01

Urinary stones are heterogeneous in their fragility to lithotripter shockwaves. As a first step in gaining a better understanding of the role of matrix in stone fragility, we measured extractible protein in calcium oxalate monohydrate (COM) stones that were extensively characterized by micro-computed tomography (micro CT). Stones were scanned using micro CT (Scanco mCT20, 34 microm). They were ground, and the protein extracted using four methods: 0.25M EDTA, 2% SDS reducing buffer, 9M urea buffer, and 10% acetic acid. Protein was measured using NanoOrange. The SDS extracts were also examined using polyacrylamide electrophoresis (PAGE). Extracted protein was highest with the SDS or urea methods (0.28% +/- 0.13% and 0.24% +/- 0.11%, respectively) and lower using the EDTA method (0.17% +/- 0.05%; P < 0.02). Acetic acid extracted little protein (0.006 +/- 0.002%; P < 0.001). Individual stones were significantly different in extractability of protein by the different methods, and SDS-PAGE revealed different protein patterns for individual stones. Extracted protein did not correlate with X-ray-lucent void percentage, which ranged from 0.06% to 2.8% of stone volume, or with apatite content. Extractible stone-matrix protein differs for individual COM stones, and yield is dependent on the extraction method. The presence of X-ray-lucent voids or minor amounts of apatite in stones did not correlate with protein content. The amounts of protein recovered were much lower than reported by Boyce, showing that these methods extracted only a fraction of the protein bound up in the stones. The results suggest that none of the methods tested will be useful for helping to answer the question of whether matrix content differs among stones of differing fragility to lithotripter shockwaves.

A validated UHPLC method for the determination of caffeoylquinic and di-caffeoylquinic acids in green coffee extracts using an RP-Amide fused-core column.

PubMed

Fibigr, Jakub; Majorová, Michaela; Kočová Vlčková, Hana; Solich, Petr; Šatínský, Dalibor

2018-03-20

The presented work describes the development and validation of a rapid UHPLC-UV method using a fused core particle column with an RP-Amide stationary phase for the separation and quantitative analysis of caffeoylquinic and di-caffeoylquinic acids in green coffee extracts. Three caffeoylquinic acids (3-caffeoylquinic acid, 4-caffeoylquinic acid, and 5-caffeoylquinic acid) and two di-caffeoylquinic acids (1,3-di-caffeoylquinic acid, and 3,5-di-caffeoylquinic acid) were separated and analyzed in 8 min. That was possible due to the unique selectivity of the RP-Amide stationary phase for the analyzed acids. The retention behavior of all analytes under different compositions of the mobile phase on different columns was evaluated in this study. The optimal chromatographic separation was performed using an Ascentis Express RP-Amide (100 × 2.1 mm) fused-core column with a particle size of 2.7 μm at a temperature of 30 °C. For validation of the newly developed method, acetonitrile was used as mobile phase B and 5% formic acid, filtrated through a 0.22 μm filter, was used as mobile phase A. They were delivered at a flow rate of 0.9 mL min -1 according to the elution gradient program. The detection wavelength was set at 325 nm. A solid-liquid extraction with a solution of methanol and a 5% water solution of formic acid (25 + 75 v/v) using an ultrasonic bath was chosen for the preparation of the available commercial samples of food supplements containing a green coffee extract. Recoveries for all analyzed acids were 98.2-101.0% and the relative standard deviation ranged from 0.3% to 1.4% for intra-day and from 0.3% to 3.0% for inter-day repeatability. The limits of detection were in the range of 0.30-0.53 μg mL -1 . Copyright © 2018. Published by Elsevier B.V.

A comparison of the compositional differences between humic fractions isolated by the IHSS and exhaustive extraction procedures

NASA Astrophysics Data System (ADS)

Chang, R. R.; Mylotte, R.; Hayes, M. H. B.; Mclnerney, R.; Tzou, Y. M.

2014-03-01

Humic substances (HSs), consisting, on the basis of solubilities in aqueous acid and basic media, of humic acids (HAs), fulvic acids (FAs), and humin (Hu), are the major components of soil organic matter (SOM). Most studies of soil/natural organic matter (SOM/NOM) have been carried out on extracts of soils in dilute sodium hydroxide solutions, the solvent used to extract the Standards of the International Humic Substances Society (IHSS). However, Hu, the major component in the classical definition of HSs, is insoluble in aqueous base and is not isolated by the traditional IHSS method. Recently, a sequential exhaustive extraction (SEE) process has been shown to be capable of isolating and separating the major components of the classically defined HSs from the soils of the temperate and tropical regions. The SEE system was used in the present study to isolate the HA/FA and Hu fractions from a subtropical volcanic Taiwanese soil. Chemical and compositional properties of these extracts were then compared with similarly obtained isolates from soils from the different climatic regions. Increases in the aliphatic relative to aromatic carbon contents were observed for both the HA and FA fractions when the pH values of the extraction media were increased. HAs and FAs isolated using the SEE method have spectroscopic profiles similar to those from the IHSS isolate; however, the cumulative extraction efficiency (%) of the SEE method (65 %) for the volcanic soil was much higher than for the traditional IHSS method (33 %). When the residual volcanic soil, following extractions once, three, and eight times with 0.1 M NaOH were then extracted with dimethyl sulphoxide (DMSO) plus concentrated sulphuric acid (the final solvent in the SEE sequence) it was seen that the content of crystalline polymethylene hydrocarbon (33 ppm 13C-NMR resonance in the Hu (or DMSO/acid)) extract increased relative to the amorphous methylene (30 ppm). That highlights the difficulty in dissolving the more highly ordered hydrocarbon structures that would be expected to have closer associations with the mineral colloids. Although the SEE procedure isolated all of the HAs and FAs from the Yangmingshan soil, extractability of the Hu from the volcanic soil in the DMSO/acid solvent was low (21 %), and contrasted with the much higher yields from temperate and tropical regions. The decreased Hu extraction may arise from its associations with the extensive iron and aluminium hydroxide mineral colloids in the soil. The Hu from this sub-tropical soil was different from the Hus isolated from other soil types, indicating the need to isolate and characterise these recalcitrant organic material in order to understand the organic carbon components in soils in greater detail. Such results would indicate that more attention should be given to mineral colloids in soils, and to the organo/mineral associations that will have an important role in the stabilities of OM in the soil environment.

An effective protein extraction method for two-dimensional electrophoresis in the anticancer herb Andrographis paniculata Nees.

PubMed

Talei, Daryush; Valdiani, Alireza; Puad, Mohd Abdullah

2013-01-01

Proteomic analysis of plants relies on high yields of pure protein. In plants, protein extraction and purification present a great challenge due to accumulation of a large amount of interfering substances, including polysaccharides, polyphenols, and secondary metabolites. Therefore, it is necessary to modify the extraction protocols. A study was conducted to compare four protein extraction and precipitation methods for proteomic analysis. The results showed significant differences in protein content among the four methods. The chloroform-trichloroacetic acid-acetone method using 4-(2-hydroxyethyl)-1-piperazineethanesulfonic acid (HEPES) buffer provided the best results in terms of protein content, pellets, spot resolution, and intensity of unique spots detected. An overall of 83 qualitative or quantitative significant differential spots were found among the four methods. Based on the 2-DE gel map, the method is expected to benefit the development of high-level proteomic and biochemical studies of Andrographis paniculata, which may also be applied to other recalcitrant medicinal plant tissues. © 2013 International Union of Biochemistry and Molecular Biology, Inc.

Centrifuge-less dispersive liquid-liquid microextraction base on the solidification of switchable solvent for rapid on-site extraction of four pyrethroid insecticides in water samples.

PubMed

Hu, Lu; Wang, Huazi; Qian, Heng; Liu, Chaoran; Lu, Runhua; Zhang, Sanbing; Zhou, Wenfeng; Gao, Haixiang; Xu, Donghui

2016-11-11

An on-site dispersive liquid liquid microextraction base on the solidification of switchable solvent has been developed as a simple, rapid and eco-friendly sample extraction method for the fast determination of pyrethroid insecticides in aqueous samples using high-performance liquid chromatography with ultraviolet detection. In this extraction method, medium-chain saturated fatty acids (n≥10), which can rapidly solidify at low temperatures (<20°C), were investigated as switchable hydrophilic solvents. The fatty acids were converted into the hydrophilic form by adding sodium hydroxide. Microdroplets of the fatty acids were generated when injected into an acidic sample that had been pretreated by the addition of sulfuric acid. The formed cloudy solution was cooled to a low temperature to turn the fatty acids into a solid, which was then separated by filtration, thus avoiding the time-consuming step of centrifugation. The microextraction process was performed in a 10mL syringe and the pretreatment process could thus be finished in 5min. No external energy resources were required in this method, which makes it a potential method for on-site extraction. The optimal experimental parameters were as follows: 350μL of decanoic acid (1mol/L) was used as the extraction solvent, 150μL of sulfuric acid (2mol/L) was used to decrease the pH of the samples, no salt was added, and the temperature of the samples was in the range of 20-40°C. Finally, the sample was cooled in an ice bath for three minutes. Under these optimal conditions, good responses for four pyrethroid insecticides were obtained in the concentration ranges of 1-500μg/L, with coefficients of determination greater than 0.9993. The recoveries of the four pyrethroid insecticides ranged from 84.7 to 95.3%, with relative standard deviations ranging from 1.6 to 4.6%. The limits of detection based on a signal-to-noise ratio of 3 were in the range of 0.24-0.68μg/L, and the enrichment factors were in the range of 121-136. The results demonstrate that this method was successfully applied to determine pyrethroid insecticides in real water samples. No centrifugation or any special apparatus are required, make this a promising method for rapid field-sampling procedures. Copyright © 2016 Elsevier B.V. All rights reserved.

SOLVENT EXTRACTION PROCESS FOR THE RECOVERY OF METALS FROM PHOSPHORIC ACID

DOEpatents

Bailes, R.H.; Long, R.S.

1958-11-01

> A solvent extraction process is presented for recovering metal values including uranium, thorium, and other lanthanide and actinide elements from crude industrial phosphoric acid solutions. The process conslsts of contacting said solution with an immisclble organic solvent extractant containing a diluent and a material selected from the group consisting of mono and di alkyl phosphates, alkyl phosphonates and alkyl phosphites. The uranlum enters the extractant phase and is subsequently recovered by any of the methods known to the art. Recovery is improved if the phosphate solution is treated with a reducing agent such as iron or aluminum powder prior to the extraction step.

Optimization of Extraction Conditions for Phenolic Acids from the Leaves of Melissa officinalis L. Using Response Surface Methodology

PubMed Central

Yoo, Guijae; Lee, Il Kyun; Park, Seonju; Kim, Nanyoung; Park, Jun Hyung; Kim, Seung Hyun

2018-01-01

Background: Melissa officinalis L. is a well-known medicinal plant from the family Lamiaceae, which is distributed throughout Eastern Mediterranean region and Western Asia. Objective: In this study, response surface methodology (RSM) was utilized to optimize the extraction conditions for bioactive compounds from the leaves of M. officinalis L. Materials and Methods: A Box–Behnken design (BBD) was utilized to evaluate the effects of three independent variables, namely extraction temperature (°C), methanol concentration (%), and solvent-to-material ratio (mL/g) on the responses of the contents of caffeic acid and rosmarinic acid. Results: Regression analysis showed a good fit of the experimental data. The optimal condition was obtained at extraction temperature 80.53°C, methanol concentration 29.89%, and solvent-to-material ratio 30 mL/g. Conclusion: These results indicate the suitability of the model employed and the successful application of RSM in optimizing the extraction conditions. This study may be useful for standardizing production quality, including improving the efficiency of large-scale extraction systems. SUMMARY The optimum conditions for the extraction of major phenolic acids from the leaves of Melissa officinalis L. were determined using response surface methodologyBox–Behnken design was utilized to evaluate the effects of three independent variablesQuadratic polynomial model provided a satisfactory description of the experimental dataThe optimized condition for simultaneous maximum contents of caffeic acid and rosmarinic acid was determined. Abbreviations used: RSM: Response surface methodology, BBD: Box–Behnken design, CA: Caffeic acid, RA: Rosmarinic acid, HPLC: High-performance liquid chromatography. PMID:29720824

Optimized methods for total nucleic acid extraction and quantification of the bat white-nose syndrome fungus, Pseudogymnoascus destructans, from swab and environmental samples.

PubMed

Verant, Michelle L; Bohuski, Elizabeth A; Lorch, Jeffery M; Blehert, David S

2016-03-01

The continued spread of white-nose syndrome and its impacts on hibernating bat populations across North America has prompted nationwide surveillance efforts and the need for high-throughput, noninvasive diagnostic tools. Quantitative real-time polymerase chain reaction (qPCR) analysis has been increasingly used for detection of the causative fungus, Pseudogymnoascus destructans, in both bat- and environment-associated samples and provides a tool for quantification of fungal DNA useful for research and monitoring purposes. However, precise quantification of nucleic acid from P. destructans is dependent on effective and standardized methods for extracting nucleic acid from various relevant sample types. We describe optimized methodologies for extracting fungal nucleic acids from sediment, guano, and swab-based samples using commercial kits together with a combination of chemical, enzymatic, and mechanical modifications. Additionally, we define modifications to a previously published intergenic spacer-based qPCR test for P. destructans to refine quantification capabilities of this assay. © 2016 The Author(s).

Optimized methods for total nucleic acid extraction and quantification of the bat white-nose syndrome fungus, Pseudogymnoascus destructans, from swab and environmental samples

USGS Publications Warehouse

Verant, Michelle; Bohuski, Elizabeth A.; Lorch, Jeffrey M.; Blehert, David

2016-01-01

The continued spread of white-nose syndrome and its impacts on hibernating bat populations across North America has prompted nationwide surveillance efforts and the need for high-throughput, noninvasive diagnostic tools. Quantitative real-time polymerase chain reaction (qPCR) analysis has been increasingly used for detection of the causative fungus, Pseudogymnoascus destructans, in both bat- and environment-associated samples and provides a tool for quantification of fungal DNA useful for research and monitoring purposes. However, precise quantification of nucleic acid fromP. destructans is dependent on effective and standardized methods for extracting nucleic acid from various relevant sample types. We describe optimized methodologies for extracting fungal nucleic acids from sediment, guano, and swab-based samples using commercial kits together with a combination of chemical, enzymatic, and mechanical modifications. Additionally, we define modifications to a previously published intergenic spacer–based qPCR test for P. destructans to refine quantification capabilities of this assay.

METHOD FOR THE RECOVERY AND PURIFICATION OF BERKELIUM

DOEpatents

Hulet, E.K.

1959-10-20

A solvent extraction process is described for the separation of berkelium from a mixture of elements in the lanthanum and actinium series of the periodic table. In particular, the mixture of elements is dissolved in 1.0N nitric acid, and the resulting solution is extracted with n-tributyl phosphate containlng a stoichiometric excess of solid sodium bismuthate. The berkelium present in the nitric acid solution is oxidized to the IV oxidation state and is preferentially- extracted into the n-tributyl phosphate. The organic phase, containing berkelium in an oxidized state, is extracted with 0.1N hydrochloric acid solution containing a small quantity- of a reducing agent such as yvdrazine hydrochloride. The berkelium is reduced to the III oxidation state and is extracted into the aqueous phase. The berkelium is then recovered from the aqueous phase.

Healing and Antisecretory Effects of Aqueous Extract of Eremomastax speciosa (Acanthaceae) on Unhealed Gastric Ulcers

PubMed Central

Amang, A. P.; Mezui, C.; Siwe, G. T.; Emakoua, J.; Mbah, G.; Nkwengoua, E. Z.; Enow-Orock, G. E.

2017-01-01

Objective This work investigated the healing and antisecretory effects of the aqueous extract of Eremomastax speciosa on “unhealed gastric ulcers” associated with gastric acid hypersecretion. Materials and Methods “Unhealed gastric ulcers” were induced using indomethacin following the establishment of acetic-acid-induced chronic gastric ulcers. The extract (200 and 400 mg/kg, per os) was administered concomitantly with indomethacin (1 mg/kg, subcutaneously). The effects of the extract on both basal and histamine-stimulated gastric acid secretion were determined. Mucus secretion and oxidative stress parameters were measured, and histological assessment of ulcer healing was carried out. Results The extract significantly promoted the healing process in rats subjected to “unhealed gastric ulcers” (82.4–88.5% healing rates). Treatment with the extract significantly reduced the basal (25.95–49.51% reduction rates) and histamine-stimulated (24.25–47.41%) acid secretions. The healing effect of the extract was associated with a significant (p < 0.05) increase of mucus secretion and concentrations of antioxidant enzymes compared with the controls. The extract at the highest dose showed normalization of the mucosa, without glandular destruction and with the disappearance of fibrosis and lymphocyte infiltration. Conclusion The abilities of the extract to increase mucus secretion, to reinforce antioxidant status, and to inhibit acid secretion would be some of the mechanisms by which this extract would accelerate the healing process in “unhealed gastric ulcers.” PMID:29234676

Comparison of the acetyl bromide spectrophotometric method with other analytical lignin methods for determining lignin concentration in forage samples.

PubMed

Fukushima, Romualdo S; Hatfield, Ronald D

2004-06-16

Present analytical methods to quantify lignin in herbaceous plants are not totally satisfactory. A spectrophotometric method, acetyl bromide soluble lignin (ABSL), has been employed to determine lignin concentration in a range of plant materials. In this work, lignin extracted with acidic dioxane was used to develop standard curves and to calculate the derived linear regression equation (slope equals absorptivity value or extinction coefficient) for determining the lignin concentration of respective cell wall samples. This procedure yielded lignin values that were different from those obtained with Klason lignin, acid detergent acid insoluble lignin, or permanganate lignin procedures. Correlations with in vitro dry matter or cell wall digestibility of samples were highest with data from the spectrophotometric technique. The ABSL method employing as standard lignin extracted with acidic dioxane has the potential to be employed as an analytical method to determine lignin concentration in a range of forage materials. It may be useful in developing a quick and easy method to predict in vitro digestibility on the basis of the total lignin content of a sample.

Quantitative extraction and concentration of synthetic water-soluble acid dyes from aqueous media using a quinine-chloroform solution

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kobayashi, F.; Ozawa, N.; Hanai, J.

Twenty-one water-soluble acid dyes, including eleven azo, five triphenylmethane four xanthene, one naphthol derivatives, used at practical concentrations for food coloration, were quantitatively extracted from water and various carbonated beverages into a 0.1 M quinine-chloroform solution in the presence of 0.5 M boric acid by brief shaking. Quantitative extraction of these dyes was also accomplished by the 0.1 M quinine-chloroform solution made conveniently from chloroform, quinine hydrochloride, and sodium hydroxide added successively to water or beverages containing boric acid. Quinine acted as a countercation on the dyes having sulfonic and/or carboxylic acid group(s) to form chloroform-soluble ion-pair complexes. The diacidicmore » base alkaloid interacted with each acid group of mono-, di-, tri-, and tetrasulfonic acid dyes approximately in the ratio 0.8-0.9 to 1. The dyes in the chloroform solution were quantitatively concentrated into a small volume of sodium hydroxide solution also by brief shaking. The convenient quinine-chloroform method was applicable to the quantitative extraction of a mixture of 12 dyes from carbonated beverages, which are all currently used for food coloration. A high-pressure liquid chromatographic method is also presented for the systematic separation and determination of these 12 dyes following their concentration into the aqueous alkaline solution. The chromatogram was monitored by double-wavelength absorptiometry in the visible and ultraviolet ray regions.« less

[Pharmacological study on hemostasis, analgesic and anti inflammation effects of the alcohol extract of Hibiscus tiliaceus].

PubMed

Qiu, Fen; Tian, Hui; Zhang, Zhi; Yuan, Xian-Ling; Tan, Yuan-Feng; Ning, Xiao-Qing

2013-10-01

To study the effects of hemostasis, analgesic and anti inflammation of the alcohol extract of Hibiscus tiliaceus and offer pharmacological and experimental basis for its safe and effective use in clinic. The effects of hemostasist were observed with tail breaking method, capillary tube method and slide method; Hot board and body distortion induced by acetic acid methods were applied in mice analgesia experiment, the mice model of acute auricle swelling induced by dmi ethylbenzene and capillary permeability induced by acetic acid were applied to observe the anti inflammatory effects. The alcohol extract of Hibiscus tiliaceus could significantly reduce the bleeding time and the clotting time, delay the plant reaction time and reduce the writhing times of the mice, and it also had effect on inhibiting swelling of mice ear and the permeability of the capillary. These results suggest that the alcohol extract of Hibiscus tiliaceus has the effects of hemostasis, analgesic and anti inflammation.

Sampling and analysis of airborne resin acids and solvent-soluble material derived from heated colophony (rosin) flux: a method to quantify exposure to sensitizing compounds liberated during electronics soldering.

PubMed

Smith, P A; Son, P S; Callaghan, P M; Jederberg, W W; Kuhlmann, K; Still, K R

1996-07-17

Components of colophony (rosin) resin acids are sensitizers through dermal and pulmonary exposure to heated and unheated material. Significant work in the literature identifies specific resin acids and their oxidation products as sensitizers. Pulmonary exposure to colophony sensitizers has been estimated indirectly through formaldehyde exposure. To assess pulmonary sensitization from airborne resin acids, direct measurement is desired, as the degree to which aldehyde exposure correlates with that of resin acids during colophony heating is undefined. Any analytical method proposed should be applicable to a range of compounds and should also identify specific compounds present in a breathing zone sample. This work adapts OSHA Sampling and Analytical Method 58, which is designed to provide airborne concentration data for coal tar pitch volatile solids by air filtration through a glass fiber filter, solvent extraction of the filter, and gravimetric analysis of the non-volatile extract residue. In addition to data regarding total soluble material captured, a portion of the extract may be subjected to compound-specific analysis. Levels of soluble solids found during personal breathing zone sampling during electronics soldering in a Naval Aviation Depot ranged from below the "reliable quantitation limit" reported in the method to 7.98 mg/m3. Colophony-spiked filters analyzed in accordance with the method (modified) produced a limit of detection for total solvent-soluble colophony solids of 10 micrograms/filter. High performance liquid chromatography was used to identify abietic acid present in a breathing zone sample.

Preparation of hybrid molecularly imprinted polymer with double-templates for rapid simultaneous purification of theophylline and chlorogenic acid in green tea.

PubMed

Tang, Weiyang; Li, Guizhen; Row, Kyung Ho; Zhu, Tao

2016-05-15

A novel double-templates technique was adopted for solid-phase extraction packing agent, and the obtained hybrid molecularly imprinted polymers with double-templates (theophylline and chlorogenic acid) were characterized by fourier transform infrared and field emission scanning electron microscope. The molecular recognition ability and binding capability for theophylline and chlorogenic acid of polymers was evaluated by static absorption and dynamic adsorption curves. A rapid and accurate approach was established for simultaneous purification of theophylline and chlorogenic acid in green tea by coupling hybrid molecularly imprinted solid-phase extraction with high performance liquid chromatography. With optimization of SPE procedure, a reliable analytical method was developed for highly recognition towards theophylline and chlorogenic acid in green tea with satisfactory extraction recoveries (theophylline: 96.7% and chlorogenic acid: 95.8%). The limit of detection and limit of quantity of the method were 0.01 μg/mL and 0.03 μg/mL for theophylline, 0.05 μg/mL and 0.17 μg/mL for chlorogenic acid, respectively. The recoveries of proposed method at three spiked levels analysis were 98.7-100.8% and 98.3-100.2%, respectively, with the relative standard deviation less than 1.9%. Hybrid molecularly imprinted polymers with double-templates showed good performance for two kinds of targets, and the proposed approach with high affinity of hybrid molecularly imprinted polymers might offer a novel method for the purification of complex samples. Copyright © 2016 Elsevier B.V. All rights reserved.

Obtaining a Dry Extract from the Mikania laevigata Leaves with Potential for Antiulcer Activity

PubMed Central

Pinto, Mariana Viana; Oliveira, Ezequiane Machado; Martins, Jose Luiz Rodrigues; de Paula, Jose Realino; Costa, Elson Alves; da Conceição, Edemilson Cardoso; Bara, Maria Teresa Freitas

2017-01-01

Background: Mikania laevigata leaves are commonly used in Brazil as a medicinal plant. Objective: To obtain hydroalcoholic dried extract by nebulization and evaluate its antiulcerogenic potential. Materials and Methods: Plant material and hydroalcoholic extract were processed and analyzed for their physicochemical characteristics. A method using HPLC was validated to quantify coumarin and o-coumaric acid. Hydroalcoholic extract was spray dried and the powder obtained was characterized in terms of its physicochemical parameters and potential for antiulcerogenic activity. Results: The analytical method proved to be selective, linear, precise, accurate, sensitive, and robust. M. laevigata spray dried extract was obtained using colloidal silicon dioxide as adjuvant and was shown to possess 1.83 ± 0.004% coumarin and 0.80 ± 0.012% o-coumaric acid. It showed significant antiulcer activity in a model of an indomethacin-induced gastric lesion in mice and also produced a gastroprotective effect. Conclusion: This dried extract from M. laevigata could be a promising intermediate phytopharmaceutical product. SUMMARY Research and development of standardized dried extract of Mikania laevigata leaves obtained through spray drying and the production process was monitored by the chemical profile, physicochemical properties and potential for anti-ulcerogenic activity. Abbreviations used: DE: M. laevigata spray dried extract, HE: hydroalcoholic extract. PMID:28216886

Simultaneous quantification of the major bile acids in artificial Calculus bovis by high-performance liquid chromatography with precolumn derivatization and its application in quality control.

PubMed

Shi, Yan; Xiong, Jing; Sun, Dongmei; Liu, Wei; Wei, Feng; Ma, Shuangcheng; Lin, Ruichao

2015-08-01

An accurate and sensitive high-performance liquid chromatography method coupled with ultralviolet detection and precolumn derivatization was developed for the simultaneous quantification of the major bile acids in Artificial Calculus bovis, including cholic acid, hyodeoxycholic acid, chenodeoxycholic acid, and deoxycholic acid. The extraction, derivatization, chromatographic separation, and detection parameters were fully optimized. The samples were extracted with methanol by ultrasonic extraction. Then, 2-bromine-4'-nitroacetophenone and 18-crown ether-6 were used for derivatization. The chromatographic separation was performed on an Agilent SB-C18 column (250 × 4.6 mm id, 5 μm) at a column temperature of 30°C and liquid flow rate of 1.0 mL/min using water and methanol as the mobile phase with a gradient elution. The detection wavelength was 263 nm. The method was extensively validated by evaluating the linearity (r(2) ≥ 0.9980), recovery (94.24-98.91%), limits of detection (0.25-0.31 ng) and limits of quantification (0.83-1.02 ng). Seventeen samples were analyzed using the developed and validated method. Then, the amounts of bile acids were analyzed by hierarchical agglomerative clustering analysis and principal component analysis. The results of the chemometric analysis showed that the contents of these compounds reflect the intrinsic quality of artificial Calculus bovis, and two compounds (hyodeoxycholic acid and chenodeoxycholic acid) were the most important markers for quality evaluating. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Detection of malondialdehyde in processed meat products without interference from the ingredients.

PubMed

Jung, Samooel; Nam, Ki Chang; Jo, Cheorun

2016-10-15

Our aim was to develop a method for accurate quantification of malondialdehyde (MDA) in meat products. MDA content of uncured ground pork (Control); ground pork cured with sodium nitrite (Nitrite); and ground pork cured with sodium nitrite, sodium chloride, sodium pyrophosphate, maltodextrin, and a sausage seasoning (Mix) was measured by the 2-thiobarbituric acid (TBA) assay with MDA extraction by trichloroacetic acid (method A) and two high-performance liquid chromatography (HPLC) methods: i) HPLC separation of the MDA-dinitrophenyl hydrazine adduct (method B) and ii) HPLC separation of MDA (method C) after MDA extraction with acetonitrile. Methods A and B could not quantify MDA accurately in groups Nitrite and Mix. Nevertheless, MDA in groups Control, Nitrite, and Mix was accurately quantified by method C with good recovery. Therefore, direct MDA quantification by HPLC after MDA extraction with acetonitrile (method C) is useful for accurate measurement of MDA content in processed meat products. Copyright © 2016 Elsevier Ltd. All rights reserved.

Antiproliferative effect of methanolic extraction of tualang honey on human keloid fibroblasts

PubMed Central

2011-01-01

Background Keloid is a type of scar which extends beyond the boundaries of the original wound. It can spread to the surrounding skin by invasion. The use of Tualang honey is a possible approach for keloid treatment. The objective of this study was to determine the antiproliferative effect of methanolic extraction of Tualang honey to primary human keloid fibroblasts and to identify the volatile compounds in methanol extraction of Tualang honey. Methods Crude Tualang honey was extracted with methanol and then dried using rota vapor to remove remaining methanol from honey. Normal and keloid fibroblasts were verified and treated with the extracted honey. Cell proliferation was tested with [3-(4,5-dimethylthiazol-2-yi)-5-(3-carboxymethoxyphenyl)-2-(4-sulfophenyl)-2H-tetrazolium, inner salt] (MTS) assay. Extraction of Tualang honey using methanol was carried out and the extracted samples were analysed using gas chromatography-mass spectrometry (GC-MS). The result was analysed using SPSS and tested with Kruskal-Wallis and Mann-Whitney tests. Results Methanolic extraction of honey has positive anti proliferative effect on keloid fibroblasts in a dose-dependent manner. The presence of fatty acids such as palmitic acid, stearic acid, oleic acid, linoleic acid and octadecanoic acid may contribute to the anti-proliferative effect in keloid fibroblasts. Conclusions The methanolic honey extraction has an antiproliferative effect on keloid fibroblasts and a range of volatile compounds has been identified from Tualang honey. The antiproliferative effect of keloid fibroblasts towards Tualang honey may involve cell signaling pathway. Identifying other volatile compounds from different organic solvents should be carried out in future. PMID:21943200

Extraction and the Fatty Acid Profile of Rosa acicularis Seed Oil.

PubMed

Du, Huanan; Zhang, Xu; Zhang, Ruchun; Zhang, Lu; Yu, Dianyu; Jiang, Lianzhou

2017-12-01

Rosa acicularis seed oil was extracted from Rosa acicularis seeds by the ultrasonic-assisted aqueous enzymatic method using cellulase and protease. Based on a single experiment, Plackett-Burman design was applied to ultrasonic-assisted aqueous enzymatic extraction of wild rose seed oil. The effects of enzyme amount, hydrolysis temperature and initial pH on total extraction rate of wild rose seed oil was studied by using Box-Behnken optimize methodology. Chemical characteristics of a sample of Rosa acicularis seeds and Rosa acicularis seed oil were characterized in this work. The tocopherol content was 200.6±0.3 mg/100 g oil. The Rosa acicularis seed oil was rich in linoleic acid (56.5%) and oleic acid (34.2%). The saturated fatty acids included palmitic acid (4%) and stearic acid (2.9%). The major fatty acids in the sn-2 position of triacylglycerol in Rosa acicularis oil were linoleic acid (60.6%), oleic acid (33.6%) and linolenic acid (3.2%). According to the 1,3-random-2-random hypothesis, the dominant triacylglycerols were LLL (18%), LLnL (1%), LLP (2%), LOL (10%), LLSt (1.2%), PLP (0.2%), LLnP (0.1%), LLnO (0.6%) and LOP (1.1%). This work could be useful for developing applications for Rosa acicularis seed oil.

Extraction fatty acid as a source to produce biofuel in microalgae Chlorella sp. and Spirulina sp. using supercritical carbon dioxide

NASA Astrophysics Data System (ADS)

Tai, Do Chiem; Hai, Dam Thi Thanh; Vinh, Nguyen Hanh; Phung, Le Thi Kim

2016-06-01

In this research, the fatty acids of isolated microalgae were extracted by some technologies such as maceration, Soxhlet, ultrasonic-assisted extraction and supercritical fluid extraction; and analyzed for biodiesel production using GC-MS. This work deals with the extraction of microalgae oil from dry biomass by using supercritical fluid extraction method. A complete study at laboratory of the influence of some parameters on the extraction kinetics and yields and on the composition of the oil in terms of lipid classes and profiles is proposed. Two types of microalgae were studied: Chlorella sp. and Spirulina sp. For the extraction of oil from microalgae, supercritical CO2 (SC-CO2) is regarded with interest, being safer than n-hexane and offering a negligible environmental impact, a short extraction time and a high-quality final product. Whilst some experimental papers are available on the supercritical fluid extraction (SFE) of oil from microalgae, only limited information exists on the kinetics of the process. These results demonstrate that supercritical CO2 extraction is an efficient method for the complete recovery of the neutral lipid phase.

Two-Stage Separation of V(IV) and Al(III) by Crystallization and Solvent Extraction from Aluminum-Rich Sulfuric Acid Leaching Solution of Stone Coal

NASA Astrophysics Data System (ADS)

Shi, Qihua; Zhang, Yimin; Liu, Tao; Huang, Jing; Liu, Hong

2017-10-01

To improve separation of V(IV) and Al(III) from aluminum-rich sulfuric acid leaching solution of stone coal, the two-stage separation by crystallization and solvent extraction methods have been developed. A co-extraction coefficient ( k) was put forward to evaluate comprehensively co-extraction extent in different solutions. In the crystallization stage, 68.2% of aluminum can be removed from the solution. In the solvent extraction stage, vanadium was selectively extracted using di-2-ethylhexyl phosphoric acid/tri-n-butyl phosphate from the crystalline mother solution, followed by H2SO4 stripped efficiently. A V2O5 product with purity of 98.39% and only 0.10% Al was obtained after oxidation, precipitation, and calcination. Compared with vanadium extraction from solution without crystallization, the counter-current extraction stage of vanadium can be decreased from 6 to 3 and co-extraction coefficient ( k) decreased from 2.51 to 0.58 with two-stage separation. It is suggested that the aluminum removal by crystallization can evidently weaken the influence of aluminum co-extraction on vanadium extraction and improve the selectivity of solvent extraction for vanadium.

A green deep eutectic solvent dispersive liquid-liquid micro-extraction (DES-DLLME) for the UHPLC-PDA determination of oxyprenylated phenylpropanoids in olive, soy, peanuts, corn, and sunflower oil.

PubMed

Ferrone, Vincenzo; Genovese, Salvatore; Carlucci, Maura; Tiecco, Matteo; Germani, Raimondo; Preziuso, Francesca; Epifano, Francesco; Carlucci, Giuseppe; Taddeo, Vito Alessandro

2018-04-15

A green dispersive liquid-liquid microextraction (DLLME) using deep eutectic solvent (DES) as the extracting solvent has been developed and applied for the simultaneous quantification of ferulic acid, umbelliferone, boropinic acid, 7-isopentenyloxycoumarin, 4'-geranyloxyferulic acid (GOFA), and auraptene in some vegetable oils using ultra high performance liquid chromatography (UHPLC) with photodiode array detection (PDA). All parameters in the extraction step, including selection and loading of both extracting and dispersing solvents, amount of both extractant and disperser solvent were investigated and optimized. PhAA/TMG DES achieved higher recovery and enrichment factor compared to other DESs. The validated method showed good linearity with correlation coefficients, r 2 >0.9990 for all the analytes. Furthermore, this is the first time that eco-friendly solvents are used for the extraction of oxyprenylated phenylpropanoids and the corresponding extract analyzed with ultra high performance liquid chromatography with photodiode array detection. Copyright © 2017 Elsevier Ltd. All rights reserved.

Extraction of polyphenols from processed black currant (Ribes nigrum L.) residues.

PubMed

Kapasakalidis, Petros G; Rastall, Robert A; Gordon, Michael H

2006-05-31

The total phenol and anthocyanin contents of black currant pomace and black currant press residue (BPR) extracts, extracted with formic acid in methanol or with methanol/water/acetic acid, were studied. Anthocyanins and other phenols were identified by means of reversed phase HPLC, and differences between the two plant materials were monitored. In all BPR extracts, phenol levels, determined by the Folin-Ciocalteu method, were 8-9 times higher than in the pomace extracts. Acid hydrolysis liberated a much higher concentration of phenols from the pomace than from the black currant press residue. HPLC analysis revealed that delphinidin-3-O-glucoside, delphinidin-3-O-rutinoside, cyanidin-3-O-glucoside, and cyanidin-3-O-rutinoside were the major anthocyanins and constituted the main phenol class ( approximately 90%) in both types of black currant tissues tested. However, anthocyanins were present in considerably lower amounts in the pomace than in the BPR. In accordance with the total phenol content, the antioxidant activity determined by scavenging of 2,2'-azinobis(3-ethylbenzothiazoline-6-sulfonic acid) radical cation, the ABTS(*)(+) assay, showed that BPR extracts prepared by solvent extraction exhibited significantly higher (7-10 times) radical scavenging activity than the pomace extracts, and BPR anthocyanins contributed significantly (74 and 77%) to the observed high radical scavenging capacity of the corresponding extracts.

Three phases hollow fiber LPME combined with HPLC-UV for extraction, preconcentration and determination of valerenic acid in Valeriana officinalis.

PubMed

Mirzaei, Mohamad; Dinpanah, Hossein

2011-07-01

In the present work, the applicability of hollow fiber-based liquid phase microextraction (HF-LPME) was evaluated for the extraction and preconcentration of valerenic acid prior to its determination by reversed-phase HPLC/UV. The target drug was extracted from 5.0 mL of aqueous solution with pH 3.5 into an organic extracting solvent (dihexyl ether) impregnated in the pores of a hollow fiber and finally back extracted into 10 μ L of aqueous solution with pH 9.5 located inside the lumen of the hollow fiber. In order to obtain high extraction efficiency, the parameters affecting the HF-LPME, including pH of the donor and acceptor phases, type of organic phase, ionic strength, the volume ratio of donor to acceptor phase, stirring rate and extraction time were studied and optimized. Under the optimized conditions, enrichment factor up to 446 was achieved and the relative standard deviation (RSD) of the method was 4.36% (n = 9). The linear range was 7.5-850 μg L⁻¹ with correlation coefficient (r²=0.999), detection limits was 2.5 μg L⁻¹ and the LOQ was 7.5 μg L⁻¹. The proposed method was evaluated by extraction and determination of valerenic acid in some Iranian wild species of Valerianaceae. Copyright © 2011 Elsevier B.V. All rights reserved.

Rapid and sensitive determination of major polyphenolic components in Euphoria longana Lam. seeds using matrix solid-phase dispersion extraction and UHPLC with hybrid linear ion trap triple quadrupole mass spectrometry.

PubMed

Rathore, Atul S; Sathiyanarayanan, L; Deshpande, Shreekant; Mahadik, Kakasaheb R

2016-11-01

A rapid and sensitive method for the extraction and determination of four major polyphenolic components in Euphoria longana Lam. seeds is presented for the first time based on matrix solid-phase dispersion extraction followed by ultra high performance liquid chromatography with hybrid triple quadrupole linear ion trap mass spectrometry. Matrix solid-phase dispersion method was designed for the extraction of Euphoria longana seed constituents and compared with microwave-assisted extraction and ultrasonic-assisted extraction methods. An Ultra high performance liquid chromatography with hybrid triple quadrupole linear ion-trap mass spectrometry method was developed for quantitative analysis in multiple-reaction monitoring mode in negative electrospray ionization. The chromatographic separation was accomplished using an ACQUITY UPLC BEH C 18 (2.1 mm × 50 mm, 1.7 μm) column with gradient elution of 0.1% aqueous formic acid and 0.1% formic acid in acetonitrile. The developed method was validated with acceptable linearity (r 2 > 0.999), precision (RSD ≤ 2.22%) and recovery (RSD ≤ 2.35%). The results indicated that matrix solid-phase dispersion produced comparable extraction efficiency compared with other methods nevertheless was more convenient and time-saving with reduced requirements on sample and solvent volumes. The proposed method is rapid and sensitive in providing a promising alternative for extraction and comprehensive determination of active components for quality control of Euphoria longana products. © 2016 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

A modular method for the extraction of DNA and RNA, and the separation of DNA pools from diverse environmental sample types

PubMed Central

Lever, Mark A.; Torti, Andrea; Eickenbusch, Philip; Michaud, Alexander B.; Šantl-Temkiv, Tina; Jørgensen, Bo Barker

2015-01-01

A method for the extraction of nucleic acids from a wide range of environmental samples was developed. This method consists of several modules, which can be individually modified to maximize yields in extractions of DNA and RNA or separations of DNA pools. Modules were designed based on elaborate tests, in which permutations of all nucleic acid extraction steps were compared. The final modular protocol is suitable for extractions from igneous rock, air, water, and sediments. Sediments range from high-biomass, organic rich coastal samples to samples from the most oligotrophic region of the world's oceans and the deepest borehole ever studied by scientific ocean drilling. Extraction yields of DNA and RNA are higher than with widely used commercial kits, indicating an advantage to optimizing extraction procedures to match specific sample characteristics. The ability to separate soluble extracellular DNA pools without cell lysis from intracellular and particle-complexed DNA pools may enable new insights into the cycling and preservation of DNA in environmental samples in the future. A general protocol is outlined, along with recommendations for optimizing this general protocol for specific sample types and research goals. PMID:26042110

Graphene-sensitized microporous membrane/solvent microextraction for the preconcentration of cinnamic acid derivatives in Rhizoma Typhonii.

PubMed

Xing, Rongrong; Hu, Shuang; Chen, Xuan; Bai, Xiaohong

2014-09-01

A novel graphene-sensitized microporous membrane/solvent microextraction method named microporous membrane/graphene/solvent synergistic microextraction, coupled with high-performance liquid chromatography and UV detection, was developed and introduced for the extraction and determination of three cinnamic acid derivatives in Rhizoma Typhonii. Several factors affecting performance were investigated and optimized, including the types of graphene and extraction solvent, concentration of graphene dispersed in octanol, sample phase pH, ionic strength, stirring rate, extraction time, extraction temperature, and sample volume. Under optimized conditions, the enrichment factors of cinnamic acid derivatives ranged from 75 to 269. Good linearities were obtained from 0.01 to 10 μg/mL for all analytes with regression coefficients between 0.9927 and 0.9994. The limits of quantification were <1 ng/mL, and satisfactory recoveries (99-104%) and precision (1.1-10.8%) were also achieved. The synergistic microextraction mechanism based on graphene sensitization was analyzed and described. The experimental results showed that the method was simple, sensitive, practical, and effective for the preconcentration and determination of cinnamic acid derivatives in Rhizoma Typhonii. © 2014 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Integrated sample-to-detection chip for nucleic acid test assays.

PubMed

Prakash, R; Pabbaraju, K; Wong, S; Tellier, R; Kaler, K V I S

2016-06-01

Nucleic acid based diagnostic techniques are routinely used for the detection of infectious agents. Most of these assays rely on nucleic acid extraction platforms for the extraction and purification of nucleic acids and a separate real-time PCR platform for quantitative nucleic acid amplification tests (NATs). Several microfluidic lab on chip (LOC) technologies have been developed, where mechanical and chemical methods are used for the extraction and purification of nucleic acids. Microfluidic technologies have also been effectively utilized for chip based real-time PCR assays. However, there are few examples of microfluidic systems which have successfully integrated these two key processes. In this study, we have implemented an electro-actuation based LOC micro-device that leverages multi-frequency actuation of samples and reagents droplets for chip based nucleic acid extraction and real-time, reverse transcription (RT) PCR (qRT-PCR) amplification from clinical samples. Our prototype micro-device combines chemical lysis with electric field assisted isolation of nucleic acid in a four channel parallel processing scheme. Furthermore, a four channel parallel qRT-PCR amplification and detection assay is integrated to deliver the sample-to-detection NAT chip. The NAT chip combines dielectrophoresis and electrostatic/electrowetting actuation methods with resistive micro-heaters and temperature sensors to perform chip based integrated NATs. The two chip modules have been validated using different panels of clinical samples and their performance compared with standard platforms. This study has established that our integrated NAT chip system has a sensitivity and specificity comparable to that of the standard platforms while providing up to 10 fold reduction in sample/reagent volumes.

Determination of Perfluorocarboxylic Acids in Sludge

EPA Science Inventory

Methods were developed for the extraction from wastewater-treatment sludge and quantitation by LC/MS/MS of perfluorocarboxylic acids (PFCAs, C6 to C12), 7-3 fluorotelomer carboxylic acid (7-3 FTCA) and 8-2 fluorotelomer 2-unsaturated carboxylic acid (8-2 FTUCA) using LC/MS/MS.

ANALYSIS OF PERFLUORINATED CARBOXYLIC ACIDS IN SOILS: DETECTION AND QUANTITATION ISSUES AT LOW CONCENTRATIONS

EPA Science Inventory

Methods were developed for the extraction from soil, identification, confirmation and quantitation by LC/MS/MS of trace levels of perfluorinated octanoic acid (PFOA), perfluorinated nonanoic acid (PFNA) and perfluorinated decanoic acid (PFDA). Whereas PFOA, PFNA and PFDA all can...

The development of learning media of acid-base indicator from extract of natural colorant as an alternative media in learning chemistry

NASA Astrophysics Data System (ADS)

Nurhadi, Mukhamad; Wirhanuddin, Erwin, Muflihah, Erika, Farah; Widiyowati, Iis Intan

2017-03-01

The development of learning media of acid base indicator from extract of natural colorants as an alternative media in chemistry learning; acid-base solution by using creative problem solving model at SMA N 10 Samarinda has been done. This research aimed to create and develop the learning media from extract of natural colorants, measure its quality and effectiveness, and measure the quality of student learning outcome in acid-base solution topic by using that media. The development process used Analysis, Design, Development, Implementation, and Evaluation (ADDIE) method. The learning media of acid-base indicator was created in the form of box experiment. Its quality was in the range of very good and it was effectively applied in the learning and gave positive impact on the achievement of learning goals.

Extraction of organic acids by ion-pair formation with tri-n-octylamine. Part 7. Comparison of methods for extraction of synthetic dyes from yogurt.

PubMed

Puttemans, M L; de Voogt, M; Dryon, L; Massart, D

1985-01-01

Synthetic dyes were extracted from yogurt by different methods, but all methods had in common a liberation of dyes from the food followed by ion-pair formation with tri-n-octylamine. Extraction with pH 5.5 phosphate buffer gave high recoveries for 5 of the 7 dyes investigated and was relatively fast. Precipitation of proteins followed by polyamide adsorption and desorption gave high yields for all the dyes but was tedious and long.

Efficient purification of paclitaxel from yews using high-performance displacement chromatography technique.

PubMed

Watchueng, Jean; Kamnaing, Pierre; Gao, Jin-Ming; Kiyota, Taira; Yeboah, Faustinus; Konishi, Yasuo

2011-05-20

Paclitaxel was purified using high-performance displacement chromatography (HPDC) technique, but not by the mechanism of HPDC. On small scale, paclitaxel was extracted with methanol from dry needles of Taxus canadensis and was enriched by extracting with chloroform after removing water-soluble hydrophilic components and hexane-soluble hydrophobic components. Then, 93-99% purity of paclitaxel was obtained using the HPDC technique. On large scale, taxanes were enriched by solvent partitioning between acetic acid/MeOH/H(2)O and hexane and extracted with CH(2)Cl(2). Taxanes except paclitaxel were further removed by extracting with methanol-water-trifluoroacetic acid (1.0:98.9:0.1, v/v/v). Applying HPDC technique to water-insoluble substances is problematic as this method requires a highly aqueous solvent system. In order to overcome this incompatibility, a system was set up where paclitaxel, although in low concentration, was extracted by methanol-water-trifluoroacetic acid (10.0:89.9:0.1, v/v/v). Recycling the extracting solvent to ensure minimal volume, the extracted paclitaxel was adsorbed on a C(18) trap column. A C(18) column of 4.6mm internal diameter was then connected to the trap column. The HPDC technique was thus carried out using an isocratic acetonitrile-water-trifluoroacetic acid (30.0:69.9:0.1, v/v/v) mobile phase consisting of a displacer cetylpyridinium trifluoroacetate (3mg/mL). Paclitaxel was co-eluted with the displacer and spontaneously crystallized. The crystal (114mg) showed 99.4% purity and only 10% of paclitaxel in the starting crude extract was lost during the enrichment/purification processes. This large scale purification method was successfully applied to purify paclitaxel from Chinese yew in small scale, suggesting general applicability of the method. This is the first report of purifying a water-insoluble natural product using HPDC technique. Crown Copyright © 2011. Published by Elsevier B.V. All rights reserved.

Method development for mass spectrometry based molecular characterization of fossil fuels and biological samples

NASA Astrophysics Data System (ADS)

Mahat, Rajendra K.

In an analytical (chemical) method development process, the sample preparation step usually determines the throughput and overall success of the analysis. Both targeted and non-targeted methods were developed for the mass spectrometry (MS) based analyses of fossil fuels (coal) and lipidomic analyses of a unique micro-organism, Gemmata obscuriglobus. In the non-targeted coal analysis using GC-MS, a microwave-assisted pressurized sample extraction method was compared with the traditional extraction method, such as Soxhlet. On the other hand, methods were developed to establish a comprehensive lipidomic profile and to confirm the presence of endotoxins (a.k.a. lipopolysaccharides, LPS) in Gemmata.. The performance of pressurized heating techniques employing hot-air oven and microwave irradiation were compared with that of Soxhlet method in terms of percentage extraction efficiency and extracted analyte profiles (via GC-MS). Sub-bituminous (Powder River Range, Wyoming, USA) and bituminous (Fruitland formation, Colorado, USA) coal samples were tested. Overall 30-40% higher extraction efficiencies (by weight) were obtained with a 4 hour hot-air oven and a 20 min microwave-heating extraction in a pressurized container when compared to a 72 hour Soxhlet extraction. The pressurized methods are 25 times more economic in terms of solvent/sample amount used and are 216 times faster in term of time invested for the extraction process. Additionally, same sets of compounds were identified by GC-MS for all the extraction methods used: n-alkanes and diterpanes in the sub-bituminous sample, and n-alkanes and alkyl aromatic compounds in the bituminous coal sample. G. obscuriglobus, a nucleated bacterium, is a micro-organism of high significances from evolutionary, cell and environmental biology standpoints. Although lipidomics is an essential tool in microbiological systematics and chemotaxonomy, complete lipid profile of this bacterium is still lacking. In addition, the presence of LPS and thus outer membrane (OM) in Gemmata is unknown. Global lipidomic analysis of G. obscuriglobus showed fatty acids (FAs) in the range C14 - C22, with octadecanoic and cis-9 hexadecenoic acids (C18:0 and ωc9 C16:1) being the two most abundant FAs. Thirteen different Gram-negative specific 3-hydroxy fatty acids (3-HOFAs) and eukaryote specific sterols (C30; four in number) were identified. Additionally, like a eukaryotic cell, a polyunsaturated fatty acid (PUFA; tent. ω3 C27:3) has also been discovered. The targeted lipidomic study found a series of novel biomarkers in G. obscuriglobus. Compositional analysis of LPS confirmed eight different 3-HOFAs and a sugar-acid, 2-keto 3-deoxy-D-manno -octulosonic acid (Kdo). These two groups of compounds, being unique to a Gram-negative LPS, confirmed the presence of OM in G. obscuriglobus. Moreover, compositional analyses by GC-MS also confirmed glucosamine and hexose and heptose sugars in the LPS. These compositional information obtained from GC-MS analyses were combined with molecular/structural information collected from Matrix-assisted laser desorption and ionization-time of flight (MALDI-TOF) MS. The MALDI-TOF MS showed a cluster of ions separated by 14 u, from m/z 2017.16 to 2143.28. For the most intense ion at m/z 2087.22, a tentative hexa-acylated lipid A structure has been proposed. Identifications of multiple 3-HOFAs by GC-MS and a cluster of ions in MALDI suggest presence of multiple lipid A species, i.e., heterogeneous lipid A molecule, in G. obscuriglobus..

Rapid and cost-effective determination of acrylamide in coffee by planar chromatography and fluorescence detection after derivatization with dansulfinic acid.

PubMed

Alpmann, Alexander; Morlock, Gertrud

2009-01-01

A new method has been developed for the determination of acrylamide in ground coffee by planar chromatography using prechromatographic in situ derivatization with dansulfinic acid. After pressurized fluid extraction of acrylamide from the coffee samples, the extracts were passed through activated carbon and concentrated. These extracts were applied onto a silica gel 60 HPTLC plate and oversprayed with dansulfinic acid. By heating the plate, acrylamide was derivatized into the fluorescent product dansylpropanamide. The chromatographic separation with ethyl acetate-tert.-butyl methyl ether (8 + 2, v/v) mobile phase was followed by densitometric quantification at 254/>400 nm using a 4 point calibration via the standard addition method over the whole system for which acrylamide was added at different concentrations at the beginning of the extraction process. The method was validated for commercial coffee. The linearity over the whole procedure showed determination coefficients between 0.9995 and 0.9825 (n = 6). Limit of quantitation at a signal-to-noise ratio of 10 was determined to be 48 microg/kg. The within-run precision (relative standard deviation, n = 6) of the chromatographic method was 3%. Commercial coffee samples analyzed showed acrylamide contents between 52 and 191 microg/kg, which was in correlation with amounts reported in previous publications.

Adaptogenic and nootropic activities of aqueous extract of Vitis vinifera (grape seed): an experimental study in rat model

PubMed Central

Sreemantula, Satyanarayana; Nammi, Srinivas; Kolanukonda, Rajabhanu; Koppula, Sushruta; Boini, Krishna M

2005-01-01

Background The aerial parts of Vitis vinifera (common grape or European grape) have been widely used in Ayurveda to treat a variety of common and stress related disorders. In the present investigation, the seed extract of V. vinifera was evaluated for antistress activity in normal and stress induced rats. Furthermore, the extract was studied for nootropic activity in rats and in-vitro antioxidant potential to correlate its antistress activity. Methods For the evaluation of antistress activity, groups of rats (n = 6) were subjected to forced swim stress one hour after daily treatment of V. vinifera extract. Urinary vanillylmandelic acid (VMA) and ascorbic acid were selected as non-invasive biomarkers to assess the antistress activity. The 24 h urinary excretion of vanillylmandelic acid (VMA) and ascorbic acid were determined by spectrophotometric methods in all groups under normal and stressed conditions. The nootropic activity of the extract as determined from acquisition, retention and retrieval in rats was studied by conditioned avoidance response using Cook's pole climbing apparatus. The in vitro antioxidant activity was determined based on the ability of V. vinifera to scavenge hydroxyl radicals. Results Daily administration of V. vinifera at doses of 100, 200 and 300 mg/kg body weight one hour prior to induction of stress inhibited the stress induced urinary biochemical changes in a dose dependent manner. However, no change in the urinary excretion of VMA and ascorbic acid was observed in normal animals at all the doses studied. The cognition, as determined by the acquisition, retention and recovery in rats was observed to be dose dependent. The extract also produced significant inhibition of hydroxyl radicals in comparison to ascorbic acid in a dose dependent manner. Conclusion The present study provides scientific support for the antistress (adaptogenic), antioxidant and nootropic activities of V. vinifera seed extract and substantiate the traditional claims for the usage of grape fruits and seeds in stress induced disorders. PMID:15656916

Inhibitory effect of leaves extracts of Ocimum basilicum and Ocimum gratissimum on two key enzymes involved in obesity and hypertension in vitro

PubMed Central

Irondi, Emmanuel Anyachukwu; Agboola, Samson Olalekan; Oboh, Ganiyu; Boligon, Aline Augusti

2016-01-01

Aim: To evaluate the phenolics composition and inhibitory effect of the leaves extracts of Ocimum basilicum and Ocimum gratissimum on two key enzymes (pancreatic lipase [PL] and angiotensin 1-converting enzyme [ACE]) involved in obesity and hypertension in vitro. Materials and Methods: The phenolics (flavonoids and phenolic acids) were quantified using high-performance liquid chromatography coupled with diode array detection. PL and ACE inhibitory effects; DPPH* and ABTS*+ scavenging activities of the extracts were tested using spectrophotometric methods. Results: O. basilicum had the following major phenolics: Rutin, quercetin, and quercitrin (flavonoids); caffeic, chlorogenic, and gallic acids (phenolic acids); while O. gratissimum had the following major phenolics: Rutin, quercitrin, and luteolin (flavonoids); ellagic and chlorogenic acids (phenolic acids). “Extracts of both plants inhibited PL and ACE; scavenged DPPH* in a dose-dependent manner”. O. gratissimum extract was more potent in inhibiting PL (IC50: 20.69 µg/mL) and ACE (IC50: 29.44 µg/mL) than O. basilicum (IC50: 52.14 µg/mL and IC50: 64.99 µg/mL, against PL and ACE, respectively). O. gratissimum also scavenged DPPH* and ABTS*+ more than O. basilicum. Conclusion: O. basilicum and O. gratissimum leaves could be used as functional foods for the management of obesity and obesity-related hypertension. However, O. gratissimum may be more effective than O. basilicum. PMID:27757270

Electrogeochemical sampling with NEOCHIM - results of tests over buried gold deposits

USGS Publications Warehouse

Leinz, R.W.; Hoover, D.B.; Fey, D.L.; Smith, D.B.; Patterson, T.

1998-01-01

Electrogeochemical extraction methods are based on the migration of ions in an electric field. Ions present in soil moisture are transported by an applied current into fluids contained in special electrodes placed on the soil. The fluids are then collected and analyzed. Extractions are governed by Faraday's and Ohm's laws and are modeled by the operation of a simple Hittord transference apparatus. Calculations show that the volume of soil sampled in an ideal electrogeochemical extraction can be orders of magnitude greater than the volumes used in more popular geochemical extraction methods, although this has not been verified experimentally. CHIM is a method of in-situ electrogeochemical extraction that was developed in the former Soviet Union and has been tested and applied internationally to exploration for buried mineral deposits. Tests carried out at the US Geological Survey (USGS) indicated that there were problems inherent in the use of CHIM technology. The cause of the problems was determined to be the diffusion of acid from the conventional electrode into the soil. The NEOCHIM electrode incorporates two compartments and a salt bridge in a design that inhibits diffusion of acid and enables the collection of anions or cations. Tests over a gold-enriched vein in Colorado and over buried, Carlin-type, disseminated gold deposits in northern Nevada show that there are similarities and differences between NEOCHIM results and those by partial extractions of soils which include simple extractions with water, dilute acids and solutions of salts used as collector fluids in the electrodes. Results of both differ from the results obtained by total chemical digestion. The results indicate that NEOCHIM responds to mineralized faults associated with disseminated gold deposits whereas partial and total chemical extraction methods do not. This suggests that faults are favored channels for the upward migration of metals and that NEOCHIM may be more effective in exploration for the deposits. It defines anomalies that are often narrow and intense, an observation previously made by CHIM researchers. The field tests show that NEOCHIM is less affected by surface contamination. A test over the Mike disseminated gold deposit indicates that the method may not be effective for locating deposits with impermeable cover. Faradaic extraction efficiencies of 20-30%, or more, are frequently achieved with NEOCHIM and the method generally shows good reproducibility, especially in extraction of major cations. However, ions of other metals that are useful in exploration, including Au and As, may be collected in low and temporally variable concentrations. The reason for this variability is unclear and requires further investigation.CHIM is a method of in-situ electrogeochemical extraction developed for the exploration of buried mineral deposits. However, electrode problems like diffusion of acid into the soil were encountered during the use of CHIM. The NEOCHIM electrode was developed to inhibit the diffusion of acid and enable collection of anions or cations. Tests over buried gold deposits showed that NEOCHIM responds to mineralized faults associated with disseminated gold deposits whereas partial and total chemical extraction methods do not. This suggests that faults are favored channels for the upward migration of metals and NEOCHIM may be effective in exploration for the deposits. But ions of metals may be collected in low and variable concentration.

Determination of Microalgal Lipid Content and Fatty Acid for Biofuel Production

PubMed Central

Chen, Zhipeng; Wang, Lingfeng

2018-01-01

Biofuels produced from microalgal biomass have received growing worldwide recognition as promising alternatives to conventional petroleum-derived fuels. Among the processes involved, the downstream refinement process for the extraction of lipids from biomass greatly influences the sustainability and efficiency of the entire biofuel system. This review summarizes and compares the current techniques for the extraction and measurement of microalgal lipids, including the gravimetric methods using organic solvents, CO2-based solvents, ionic liquids and switchable solvents, Nile red lipid visualization method, sulfo-phospho-vanillin method, and the thin-layer chromatography method. Each method has its own competitive advantages and disadvantages. For example, the organic solvents-based gravimetric method is mostly used and frequently employed as a reference standard to validate other methods, but it requires large amounts of samples and is time-consuming and expensive to recover solvents also with low selectivity towards desired products. The pretreatment approaches which aimed to disrupt cells and support subsequent lipid extraction through bead beating, microwave, ultrasonication, chemical methods, and enzymatic disruption are also introduced. Moreover, the principles and procedures for the production and quantification of fatty acids are finally described in detail, involving the preparation of fatty acid methyl esters and their quantification and composition analysis by gas chromatography.

Determination of terpenoid content in pine by organic solvent extraction and fast-GC analysis

DOE PAGES

Harman-Ware, Anne E.; Sykes, Robert; Peter, Gary F.; ...

2016-01-25

Terpenoids, naturally occurring compounds derived from isoprene units present in pine oleoresin, are a valuable source of chemicals used in solvents, fragrances, flavors, and have shown potential use as a biofuel. This paper describes a method to extract and analyze the terpenoids present in loblolly pine saplings and pine lighter wood. Various extraction solvents were tested over different times and temperatures. Samples were analyzed by pyrolysis-molecular beam mass spectrometry before and after extractions to monitor the extraction efficiency. The pyrolysis studies indicated that the optimal extraction method used a 1:1 hexane/acetone solvent system at 22°C for 1 h. Extracts frommore » the hexane/acetone experiments were analyzed using a low thermal mass modular accelerated column heater for fast-GC/FID analysis. The most abundant terpenoids from the pine samples were quantified, using standard curves, and included the monoterpenes, α- and β-pinene, camphene, and δ-carene. Sesquiterpenes analyzed included caryophyllene, humulene, and α-bisabolene. In conclusion, diterpenoid resin acids were quantified in derivatized extractions, including pimaric, isopimaric, levopimaric, palustric, dehydroabietic, abietic, and neoabietic acids.« less

Antibacterial properties of the skin mucus of the freshwater fishes, Rita rita and Channa punctatus.

PubMed

Kumari, U; Nigam, A K; Mitial, S; Mitial, A K

2011-07-01

The skin mucus of Rita rita and Channa punctatus was investigated to explore the possibilities of its antibacterial properties. Skin mucus was extracted in acidic solvents (0.1% trifluoroacetic acid and 3% acetic acid) and in triple distilled water (aqueous medium). The antibacterial activity of the mucus extracts was analyzed, using disc diffusion method, against five strains of bacteria--the Gram-positive Staphylococcus aureus and Micrococcus luteus; and the Gram negative Escherichia coli, Pseudomonas aeruginosa and Salmonella typhi. In both Rita rita and Channa punctatus, the skin mucus extracted in acidic solvents as well as in aqueous medium show antibacterial activity against Staphylococcus aureus and Micrococcus luteus. Nevertheless, the activity is higher in acidic solvents than that in aqueous medium. The acidic mucus extracts of Rita rita, show antibacterial activity against Salmonella typhi as well. The results suggest that fish skin mucus have bactericidal properties and thus play important role in the protection of fish against the invasion of pathogens. Fish skin mucus could thus be regarded as a potential source of novel antibacterial components.

Fuel agglomerates and method of agglomeration

DOEpatents

Wen, Wu-Wey

1986-01-01

Solid fuel agglomerates are prepared of particulate coal or other carbonaceous material with a binder having a high humic acid or humate salt content. The humic acid is extracted from oxidized carbonaceous material with a mild aqueous alkali solution of, for instance, ammonia. The particulate material is blended with the extract which serves as the binder for the agglomerates. The water-resistant agglomerates are formed such as by pelletizing, followed by drying to remove moisture and solidify the humic acid binder throughout the agglomerate.

Optimized Extraction Method To Remove Humic Acid Interferences from Soil Samples Prior to Microbial Proteome Measurements.

PubMed

Qian, Chen; Hettich, Robert L

2017-07-07

The microbial composition and their activities in soil environments play a critical role in organic matter transformation and nutrient cycling. Liquid chromatography coupled to high-performance mass spectrometry provides a powerful approach to characterize soil microbiomes; however, the limited microbial biomass and the presence of abundant interferences in soil samples present major challenges to proteome extraction and subsequent MS measurement. To this end, we have designed an experimental method to improve microbial proteome measurement by removing the soil-borne humic substances coextraction from soils. Our approach employs an in situ detergent-based microbial lysis/TCA precipitation coupled to an additional cleanup step involving acidified precipitation and filtering at the peptide level to remove most of the humic acid interferences prior to proteolytic peptide measurement. The novelty of this approach is an integration to exploit two different characteristics of humic acids: (1) Humic acids are insoluble in acidic solution but should not be removed at the protein level, as undesirable protein removal may also occur. Rather it is better to leave the humics acids in the samples until the peptide level, at which point the significant differential solubility of humic acids versus peptides at low pH can be exploited very efficiently. (2) Most of the humic acids have larger molecule weights than the peptides. Therefore, filtering a pH 2 to 3 peptide solution with a 10 kDa filter will remove most of the humic acids. This method is easily interfaced with normal proteolytic processing approaches and provides a reliable and straightforward protein extraction method that efficiently removes soil-borne humic substances without inducing proteome sample loss or biasing protein identification in mass spectrometry. In general, this humic acid removal step is universal and can be adopted by any workflow to effectively remove humic acids to avoid them negatively competing with peptides for binding with reversed-phase resin or ionization in the electrospray.

[Correlation Between Functional Groups and Radical Scavenging Activities of Acidic Polysaccharides from Dendrobium].

PubMed

Liao, Ying; Yuan, Wen-yu; Zheng, Wen-ke; Luo, Ao-xue; Fan, Yi-jun

2015-11-01

To compare the radical scavenging activity of five different acidic polysaccharides, and to find the correlation with the functional groups. Alkali extraction method and Stepwise ethanol precipitation method were used to extract and concentrate the five Dendrobium polysaccharides, and to determine the contents of sulfuric acid and uronic acid of each kind of acidic polysaccharides, and the scavenging activity to ABTS+ radical and hydroxyl radical. Functional group structures were examined by FTIR Spectrometer. Five kinds of Dendrobium polysaccharides had different ability of scavenging ABTS+ free radical and hydroxyl free radical. Moreover, the study had shown that five kinds of antioxidant activity of acidic polysaccharides had obvious correlation withuronic acid and sulfuric acid. The antioxidant activity of each sample was positively correlated with the content of uronic acid, and negatively correlated with the content of sulfuric acid. Sulfuric acid can inhibit the antioxidant activity of acidic polysaccharide but uronic acid can enhance the free radical scavenging activity. By analyzing the structure characteristics of five acidic polysaccharides, all samples have similar structures, however, Dendrobium denneanum, Dendrobium devonianum and Dendrobium officinale which had β configuration have higher antioxidant activity than Dendrobium nobile and Dendrobium fimbriatum which had a configuration.

Development and Validation of HPLC Method for Determination of Crocetin, a constituent of Saffron, in Human Serum Samples

PubMed Central

Mohammadpour, Amir Hooshang; Ramezani, Mohammad; Tavakoli Anaraki, Nasim; Malaekeh-Nikouei, Bizhan; Amel Farzad, Sara; Hosseinzadeh, Hossein

2013-01-01

Objective(s): The present study reports the development and validation of a sensitive and rapid extraction method beside high performance liquid chromatographic method for the determination of crocetin in human serum. Materials and Methods: The HPLC method was carried out by using a C18 reversed-phase column and a mobile phase composed of methanol/water/acetic acid (85:14.5:0.5 v/v/v) at the flow rate of 0.8 ml/min. The UV detector was set at 423 nm and 13-cis retinoic acid was used as the internal standard. Serum samples were pretreated with solid-phase extraction using Bond Elut C18 (200mg) cartridges or with direct precipitation using acetonitrile. Results: The calibration curves were linear over the range of 0.05-1.25 µg/ml for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction. The mean recoveries of crocetin over a concentration range of 0.05-5 µg/ml serum for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction were above 70 % and 60 %, respectively. The intraday coefficients of variation were 0.37- 2.6% for direct precipitation method and 0.64 - 5.43% for solid-phase extraction. The inter day coefficients of variation were 1.69 – 6.03% for direct precipitation method and 5.13-12.74% for solid-phase extraction, respectively. The lower limit of quantification for crocetin was 0.05 µg/ml for direct precipitation method and 0.5 µg/ml for solid-phase extraction. Conclusion: The validated direct precipitation method for HPLC satisfied all of the criteria that were necessary for a bioanalytical method and could reliably quantitate crocetin in human serum for future clinical pharmacokinetic study. PMID:23638292

Evaluation of free radical scavenging and antityrosinase activities of standardized longan fruit extract.

PubMed

Rangkadilok, Nuchanart; Sitthimonchai, Somkid; Worasuttayangkurn, Luksamee; Mahidol, Chulabhorn; Ruchirawat, Mathuros; Satayavivad, Jutamaad

2007-02-01

The protective effects of fruits and vegetables against chronic diseases have been attributed to the antioxidant properties of some secondary metabolites present in these foods. Plant polyphenols have been reported to exhibit bioactive properties, and in particular antioxidant activities. Longan seeds are found to contain high levels of some beneficial polyphenolic compounds such as corilagin, gallic acid and ellagic acid. The present study examined the free radical scavenging activity of longan seed extract by using three different assay methods. Longan extracts contained corilagin ranging from zero to 50.64 mg/g DW, gallic acid from 9.18 to 23.04 mg/g DW, and ellagic acid from 8.13 to 12.65 mg/g DW depending on the cultivars. Dried longan seed extracts of cultivar Edor contained high levels of gallic acid and ellagic acid and also exhibited the highest radical scavenging activities when comparing fresh seed and dried pulp extracts. For scavenging activity of DPPH and superoxide radicals, longan seed extract was found to be as effective as Japanese green tea extract while dried longan pulp and mulberry green tea extracts showed the least scavenging activities. In the ORAC assay, both fresh and dried longan seed also had higher activity than dried pulp and whole fruit. However, the results demonstrate that three polyphenolics may not be the major contributors of the high antioxidant activity of longan water extracts but this high activity may be due to other phenolic/flavonoid glycosides and ellagitannins present in longan fruit. In addition, longan seed also showed tyrosinase inhibitory activity with IC(50) values of 2.9-3.2 mg/ml. Therefore, the preliminary observations suggest that longan seed extract could be another potential source of potent natural dietary antioxidants and also in an application as a new natural skin-whitening agent.

A robust and efficient method for the extraction of plant extracellular surface lipids as applied to the analysis of silks and seedling leaves of maize

DOE Office of Scientific and Technical Information (OSTI.GOV)

Loneman, Derek M.; Peddicord, Layton; Al-Rashid, Amani

Aerial plant organs possess a diverse array of extracellular surface lipids, including both non-polar and amphipathic constituents that collectively provide a primary line of defense against environmental stressors. Extracellular surface lipids on the stigmatic silks of maize are composed primarily of saturated and unsaturated linear hydrocarbons, as well as fatty acids, and aldehydes. To efficiently extract lipids of differing polarities from maize silks, five solvent systems (hexanes; hexanes:diethyl ether (95:5); hexanes:diethyl ether (90:10); chloroform:hexanes (1:1) and chloroform) were tested by immersing fresh silks in solvent for different extraction times. Surface lipid recovery and the relative composition of individual constituents weremore » impacted to varying degrees depending on solvent choice and duration of extraction. Analyses were performed using both silks and leaves to demonstrate the utility of the solvent- and time-optimized protocol in comparison to extraction with the commonly used chloroform solvent. Overall, the preferred solvent system was identified as hexanes:diethyl ether (90:10), based on its effectiveness in extracting surface hydrocarbons and fatty acids as well as its reduced propensity to extract presumed internal fatty acids. Metabolite profiling of wildtype and glossy1 seedlings, which are impaired in surface lipid biosynthesis, demonstrated the ability of the preferred solvent to extract extracellular surface lipids rich in amphipathic compounds (aldehydes and alcohols). In addition to the expected deficiencies in dotriacontanal and dotriacontan-1-ol for gl1 seedlings, an unexpected increase in fatty acid recovery was observed in gl1 seedlings extracted in chloroform, suggesting that chloro-form extracts lipids from internal tissues of gl1 seedlings. This highlights the importance of extraction method when evaluating mutants that have altered cuticular lipid compositions. Lastly, metabolite profiling of silks from maize inbreds B73 and Mo17, exposed to different environments and harvested at different ages, revealed differences in hydrocarbon and fatty acid composition, demonstrating the dynamic nature of surface lipid accumulation on silks.« less

A robust and efficient method for the extraction of plant extracellular surface lipids as applied to the analysis of silks and seedling leaves of maize

DOE PAGES

Loneman, Derek M.; Peddicord, Layton; Al-Rashid, Amani; ...

2017-07-11

Aerial plant organs possess a diverse array of extracellular surface lipids, including both non-polar and amphipathic constituents that collectively provide a primary line of defense against environmental stressors. Extracellular surface lipids on the stigmatic silks of maize are composed primarily of saturated and unsaturated linear hydrocarbons, as well as fatty acids, and aldehydes. To efficiently extract lipids of differing polarities from maize silks, five solvent systems (hexanes; hexanes:diethyl ether (95:5); hexanes:diethyl ether (90:10); chloroform:hexanes (1:1) and chloroform) were tested by immersing fresh silks in solvent for different extraction times. Surface lipid recovery and the relative composition of individual constituents weremore » impacted to varying degrees depending on solvent choice and duration of extraction. Analyses were performed using both silks and leaves to demonstrate the utility of the solvent- and time-optimized protocol in comparison to extraction with the commonly used chloroform solvent. Overall, the preferred solvent system was identified as hexanes:diethyl ether (90:10), based on its effectiveness in extracting surface hydrocarbons and fatty acids as well as its reduced propensity to extract presumed internal fatty acids. Metabolite profiling of wildtype and glossy1 seedlings, which are impaired in surface lipid biosynthesis, demonstrated the ability of the preferred solvent to extract extracellular surface lipids rich in amphipathic compounds (aldehydes and alcohols). In addition to the expected deficiencies in dotriacontanal and dotriacontan-1-ol for gl1 seedlings, an unexpected increase in fatty acid recovery was observed in gl1 seedlings extracted in chloroform, suggesting that chloro-form extracts lipids from internal tissues of gl1 seedlings. This highlights the importance of extraction method when evaluating mutants that have altered cuticular lipid compositions. Lastly, metabolite profiling of silks from maize inbreds B73 and Mo17, exposed to different environments and harvested at different ages, revealed differences in hydrocarbon and fatty acid composition, demonstrating the dynamic nature of surface lipid accumulation on silks.« less

Phytochemical composition and antioxidant capacity of Cordia dichotoma seeds.

PubMed

Tian, Shuge; Liu, Feng; Zhang, Xuejia; Upur, Halmuart

2014-09-01

This study aims to determine the phytochemical composition and antioxidant activity of air-dried Cordia dichotoma seeds. Total polyphenolic content was analyzed via the Folin-Ciocalteu method. Total triterpenoid content and amino acids was analyzed colorimetrically. The rosmarinic acid content was examined using high-performance liquid chromatography tandem mass spectrometry. The ethanolic extracts contained polyphenolic compounds (1.0%), triterpenoids (0.075%), amino acids (1.39%), and rosmarinic acid (0.0028%). The results from this study indicate that C. dichotoma seeds are a rich source of polyphenolic compounds and amino acids, which can be used for quality assessment. The ethanolic extract of C. dichotoma seeds has good antioxidant capacity.

Sensitive life detection strategies for low-biomass environments: optimizing extraction of nucleic acids adsorbing to terrestrial and Mars analogue minerals.

PubMed

Direito, Susana O L; Marees, Andries; Röling, Wilfred F M

2012-07-01

The adsorption of nucleic acids to mineral matrixes can result in low extraction yields and negatively influences molecular microbial ecology studies, in particular for low-biomass environments on Earth and Mars. We determined the recovery of nucleic acids from a range of minerals relevant to Earth and Mars. Clay minerals, but also other silicates and nonsilicates, showed very low recovery (< 1%). Consequently, optimization of DNA extraction was directed towards clays. The high temperatures and acidic conditions used in some methods to dissolve mineral matrices proved to destruct DNA. The most efficient method comprised a high phosphate solution (P/EtOH; 1 M phosphate, 15% ethanol buffer at pH 8) introduced at the cell-lysing step in DNA extraction, to promote chemical competition with DNA for adsorption sites. This solution increased DNA yield from clay samples spiked with known quantities of cells up to nearly 100-fold. DNA recovery was also enhanced from several mineral samples retrieved from an aquifer, while maintaining reproducible DGGE profiles. DGGE profiles were obtained for a clay sample for which no profile could be generated with the standard DNA isolation protocol. Mineralogy influenced microbial community composition. The method also proved suitable for the recovery of low molecular weight DNA (< 1.5 kb). © 2012 Federation of European Microbiological Societies. Published by Blackwell Publishing Ltd. All rights reserved.

Isolation of Abscisic Acid from Korean Acacia Honey with Anti-Helicobacter pylori Activity

PubMed Central

Kim, SeGun; Hong, InPyo; Woo, SoonOk; Jang, HyeRi; Pak, SokCheon; Han, SangMi

2017-01-01

Background: Helicobacter pylori (H. pylori) is linked to the development of the majority of peptic ulcers and some types of gastric cancers, and its antibiotic resistance is currently found worldwide. Objective: This study is aimed at evaluating the anti-H. pylori activity of Korean acacia honey and isolating the related active components using organic solvents. Material and Methods: The crude acacia honey was extracted with n-hexane, dichloromethane, ethyl acetate (EtOAc), and n-butanol. The EtOAc extract was subjected to octadecyl-silica chromatography. The extracts and fractions were then examined for anti-H. pylori activity using the agar well diffusion method. The antimicrobial activity of abscisic acid against H. pylori was investigated by determining the minimum inhibitory concentrations (MICs), minimum bactericidal concentrations (MBCs), and by performing a time-kill assay. Results: Abscisic acid related to the botanical origins of acacia honey from Korea has been analyzed using ultra-performance liquid chromatography. The MICs and MBCs of abscisic acid were 2.7 ± 1.3 and 6.9 ± 1.9 μg/mL, respectively. The bactericidal activity of abscisic acid (at 10.8 μg/mL corresponding to 4 × MIC) killed the organism within 36–72 h. These results suggest that abscisic acid isolated from Korean acacia honey has antibacterial activity against H. pylori. Conclusion: Abscisic acid isolated from Korean acacia honey can be therapeutic and may be further exploited as a potential lead candidate for the development of treatments for H. pylori-induced infections. SUMMARY The crude acacia honey was extracted with n-hexane, dichloromethane, EtOAc, and n-butanolThe EtOAc extract yielded eight fractions and four subfractions were subsequently obtained chromatographicallyAbscisic acid was isolated from one subfractionAll the solvent extracts and fractions showed antibacterial activity against H. pyloriAbscisic acid exhibited antibacterial activity against H. pylori. Abbreviations used: MeOH: Methanol; EtOAc: Ethyl acetate; TSB: Trypticase soy broth; MIC: Minimum inhibitory concentration; MBC: Minimum bactericidal concentration; CFU: Colony-forming units; UPLC: Ultra-performance liquid chromatography; DAD: Diode array detector; UV: Ultraviolet; ODS: Octadecyl-silica; MS: Mass spectrometry; SE: Standard error. PMID:28808376

Antisecretory Action of the Extract of the Aerial Parts of Eremomastax speciosa (Acanthaceae) Occurs through Antihistaminic and Anticholinergic Pathways.

PubMed

André Perfusion, Amang; Tan, Paul V; Ernestine, Nkwengoua; Barthélemy, Nyasse

2014-01-01

Objective. The objective of this study was to find out the possible antiulcer mechanism of action of Eremomastax speciosa. Method. Carbachol- and histamine-induced hypersecretion, associated with the pylorus ligation technique, were used in rats. Gastric mucosal ulceration, mucus production, pH, gastric volume, and acidity were measured. Results. Histamine and carbachol raised gastric acidity to 86.50 and 84.80 mEq/L, respectively, in the control rats, and the extracts (200 mg/kg) reduced gastric acidity to 34.60 and 39.00 mEq/L, respectively. Intraduodenal aqueous extract (400 mg/kg) in histamine- and carbachol-treated rats produced significant (P < 0.001) decreases in acid secretion to 28.50 and 28.80 mEq/L, respectively, and 100 percent inhibition of gastric ulceration. Augmented histamine-induced gastric acid secretion (90.20 mEq/L) was significantly reduced to 52.60 and 27.50 mEq/L by the 200 and 400 mg/kg doses of the aqueous extract, respectively. The extract significantly reduced (P < 0.001) the volume of gastric secretion and significantly increased mucus production. The ulcer inhibition potential of the extract significantly dropped to 25-44% (oral extract) and to 29-37% (duodenal extract) in carbachol/indomethacin-treated rats. Conclusion. The aqueous extract of E. speciosa has both cytoprotective and antisecretory effects. The antisecretory effect may involve a mechanism common to both cholinergic and histaminergic pathways.

Determination of Major Phenolic Compounds in Echinacea spp. Raw Materials and Finished Products by High-Performance Liquid Chromatography with Ultraviolet Detection: Single-Laboratory Validation Matrix Extension

PubMed Central

Brown, Paula N.; Chan, Michael; Paley, Lori; Betz, Joseph M.

2013-01-01

A method previously validated to determine caftaric acid, chlorogenic acid, cynarin, echinacoside, and cichoric acid in echinacea raw materials has been successfully applied to dry extract and liquid tincture products in response to North American consumer needs. Single-laboratory validation was used to assess the repeatability, accuracy, selectivity, LOD, LOQ, analyte stability (ruggedness), and linearity of the method, with emphasis on finished products. Repeatability precision for each phenolic compound was between 1.04 and 5.65% RSD, with HorRat values between 0.30 and 1.39 for raw and dry extract finished products. HorRat values for tinctures were between 0.09 and 1.10. Accuracy of the method was determined through spike recovery studies. Recovery of each compound from raw material negative control (ginseng) was between 90 and 114%, while recovery from the finished product negative control (maltodextrin and magnesium stearate) was between 97 and 103%. A study was conducted to determine if cichoric acid, a major phenolic component of Echinacea purpurea (L.) Moench and E. angustifolia DC, degrades during sample preparation (extraction) and HPLC analysis. No significant degradation was observed over an extended testing period using the validated method. PMID:22165004

Determination of major phenolic compounds in Echinacea spp. raw materials and finished products by high-performance liquid chromatography with ultraviolet detection: single-laboratory validation matrix extension.

PubMed

Brown, Paula N; Chan, Michael; Paley, Lori; Betz, Joseph M

2011-01-01

A method previously validated to determine caftaric acid, chlorogenic acid, cynarin, echinacoside, and cichoric acid in echinacea raw materials has been successfully applied to dry extract and liquid tincture products in response to North American consumer needs. Single-laboratory validation was used to assess the repeatability, accuracy, selectivity, LOD, LOQ, analyte stability (ruggedness), and linearity of the method, with emphasis on finished products. Repeatability precision for each phenolic compound was between 1.04 and 5.65% RSD, with HorRat values between 0.30 and 1.39 for raw and dry extract finished products. HorRat values for tinctures were between 0.09 and 1.10. Accuracy of the method was determined through spike recovery studies. Recovery of each compound from raw material negative control (ginseng) was between 90 and 114%, while recovery from the finished product negative control (maltodextrin and magnesium stearate) was between 97 and 103%. A study was conducted to determine if cichoric acid, a major phenolic component of Echinacea purpurea (L.) Moench and E. angustifolia DC, degrades during sample preparation (extraction) and HPLC analysis. No significant degradation was observed over an extended testing period using the validated method.

Ultrasound-Assisted Extraction and Identification of Natural Antioxidants from the Fruit of Melastoma sanguineum Sims.

PubMed

Zhou, Tong; Xu, Dong-Ping; Lin, Sheng-Jun; Li, Ya; Zheng, Jie; Zhou, Yue; Zhang, Jiao-Jiao; Li, Hua-Bin

2017-02-18

The fruit of Melastoma sanguineum Sims is an edible and sweet wild fruit. In our previous study, the fruit was found to have a strong antioxidant property. In this study, an ultrasound-assisted extraction (UAE) method was developed to extract natural antioxidants from the fruit of Melastoma sanguineum Sims, and a response surface methodology was used to optimize the conditions of UAE to maximize the extraction efficiency. The influence of five independent extraction parameters (ethanol concentration, solvent/material ratio, extracting time, temperature, and ultrasound power) on the extraction efficiency were investigated using a single factor experiment, and then a central composite rotatable design was used to investigate the interaction of three key parameters. The results showed that the optimal extraction conditions were 42.98% ethanol, 28.29 mL/g solvent/material ratio, 34.29 min extracting time, 60 °C temperature, and 600 W ultrasound power. Under these conditions, the Trolox equivalent antioxidant capacity (TEAC) value of the extracts was 1074.61 ± 32.56 μmol Trolox/g dry weight (DW). Compared with conventional maceration (723.27 ± 11.61 μmol Trolox/g DW) and Soxhlet extraction methods (518.37 ± 23.23 μmol Trolox/g DW), the UAE method improved the extraction efficiency, in a shorter period of time. In addition, epicatechin gallate, epicatechin, rutin, epigallocatechin, protocatechuic acid, chlorogenic acid, and quercetin, were identified and quantified in the fruit extracts of Melastoma sanguineum Sims by UPLC-MS/MS.

Simultaneous Determination of Crypto-Chlorogenic Acid, Isoquercetin, and Astragalin Contents in Moringa oleifera Leaf Extracts by TLC-Densitometric Method

PubMed Central

Vongsak, Boonyadist; Sithisarn, Pongtip; Gritsanapan, Wandee

2013-01-01

Moringa oleifera Lamarck (Moringaceae) is used as a multipurpose medicinal plant for the treatment of various diseases. Isoquercetin, astragalin, and crypto-chlorogenic acid have been previously found to be major active components in the leaves of this plant. In this study, a thin-layer-chromatography (TLC-)densitometric method was developed and validated for simultaneous quantification of these major components in the 70% ethanolic extracts of M. oleifera leaves collected from 12 locations. The average amounts of crypto-chlorogenic acid, isoquercetin, and astragalin were found to be 0.0473, 0.0427, and 0.0534% dry weight, respectively. The method was validated for linearity, precision, accuracy, limit of detection, limit of quantitation, and robustness. The linearity was obtained in the range of 100–500 ng/spot with a correlation coefficient (r) over 0.9961. Intraday and interday precisions demonstrated relative standard deviations of less than 5%. The accuracy of the method was confirmed by determining the recovery. The average recoveries of each component from the extracts were in the range of 98.28 to 99.65%. Additionally, the leaves from Chiang Mai province contained the highest amounts of all active components. The proposed TLC-densitometric method was simple, accurate, precise, and cost-effective for routine quality controlling of M. oleifera leaf extracts. PMID:23533530

Extraction of Antioxidants from Borage (Borago officinalis L.) Leaves-Optimization by Response Surface Method and Application in Oil-in-Water Emulsions.

PubMed

Segovia, Francisco; Lupo, Bryshila; Peiró, Sara; Gordon, Michael H; Almajano, María Pilar

2014-05-06

Borage (Borago officinalis L.) is a typical Spanish plant. During processing, 60% are leaves. The aim of this work is to model and optimize the extraction of polyphenol from borage leaves using the response surface method (RSM) and to use this extract for application in emulsions. The responses were: total polyphenol content (TPC), antioxidant capacity by ORAC, and rosmarinic acid by HPLC. The ranges of the variables temperature, ethanol content and time were 50-90 °C, 0%-30%-60% ethanol (v/v), and 10-15 min. For ethanolic extraction, optimal conditions were at 75.9 °C, 52% ethanol and 14.8 min, yielding activity of 27.05 mg GAE/g DW TPC; 115.96 mg TE/g DW in ORAC and 11.02 mg/L rosmarinic acid. For water extraction, optimal activity was achieved with extraction at 98.3 °C and 22 min, with responses of 22.3 mg GAE/g DW TPC; 81.6 mg TE/g DW in ORAC and 3.9 mg/L rosmarinic acid. The significant variables were ethanol concentration and temperature. For emulsions, the peroxide value was inhibited by 60% for 3% extract concentration; and 80% with 3% extract concentration and 0.2% of BSA. The p-anisidine value between the control and the emulsion with 3% extract was reduced to 73.6% and with BSA 86.3%, and others concentrations had similar behavior.

Development and Validation of HPLC Method for Determination of Crocetin, a constituent of Saffron, in Human Serum Samples.

PubMed

Mohammadpour, Amir Hooshang; Ramezani, Mohammad; Tavakoli Anaraki, Nasim; Malaekeh-Nikouei, Bizhan; Amel Farzad, Sara; Hosseinzadeh, Hossein

2013-01-01

The present study reports the development and validation of a sensitive and rapid extraction method beside high performance liquid chromatographic method for the determination of crocetin in human serum. The HPLC method was carried out by using a C18 reversed-phase column and a mobile phase composed of methanol/water/acetic acid (85:14.5:0.5 v/v/v) at the flow rate of 0.8 ml/min. The UV detector was set at 423 nm and 13-cis retinoic acid was used as the internal standard. Serum samples were pretreated with solid-phase extraction using Bond Elut C18 (200mg) cartridges or with direct precipitation using acetonitrile. The calibration curves were linear over the range of 0.05-1.25 µg/ml for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction. The mean recoveries of crocetin over a concentration range of 0.05-5 µg/ml serum for direct precipitation method and 0.5-5 µg/ml for solid-phase extraction were above 70 % and 60 %, respectively. The intraday coefficients of variation were 0.37- 2.6% for direct precipitation method and 0.64 - 5.43% for solid-phase extraction. The inter day coefficients of variation were 1.69 - 6.03% for direct precipitation method and 5.13-12.74% for solid-phase extraction, respectively. The lower limit of quantification for crocetin was 0.05 µg/ml for direct precipitation method and 0.5 µg/ml for solid-phase extraction. The validated direct precipitation method for HPLC satisfied all of the criteria that were necessary for a bioanalytical method and could reliably quantitate crocetin in human serum for future clinical pharmacokinetic study.

Structural characteristics of pumpkin pectin extracted by microwave heating.

PubMed

Yoo, Sang-Ho; Lee, Byeong-Hoo; Lee, Heungsook; Lee, Suyong; Bae, In Young; Lee, Hyeon Gyu; Fishman, Marshall L; Chau, Hoa K; Savary, Brett J; Hotchkiss, Arland T

2012-11-01

To improve extraction yield of pumpkin pectin, microwave heating was adopted in this study. Using hot acid extraction, pumpkin pectin yield decreased from 5.7% to 1.0% as pH increased from pH 1.0 to 2.0. At pH 2.5, no pectin was recovered from pumpkin flesh powder. After a pretreatment at pH 1.0 and 25 °C for 1 h, pumpkin powder was microwave-extracted at 120 °C for 3 min resulting in 10.5% of pectin yield. However, premicrowave treatment at 60 °C for 20 min did not improve extraction yield. When microwave heating at 80 °C for 10 min was applied after premicrowave treatment, final pectin yield increased to 11.3%. When pH was adjusted to 2.0, the yield dropped to 7.7% under the same extraction conditions. Molecular shape and properties as well as chemical composition of pumpkin pectin were significantly affected depending on extraction methods. Galacturonic acid content (51% to 58%) of pumpkin pectin was lower than that detected in commercial acid-extracted citrus pectin, while higher content of neutral sugars and acetyl esters existed in pumpkin pectin structure. Molecular weight (M(w) ) and intrinsic viscosity (η(w) ) determined for microwave-extracted pumpkin pectins were substantially lower than acid-extracted pectin, whereas polydispersity was greater. However, microwave-extracted pectin at pH 2.0 had more than 5 times greater M(w) than did the pectin extracted at pH 1.0. The η(w) of microwave-extracted pectin produced at pH 2.0 was almost twice that of other microwave-extracted pectins, which were comparable to that of acid-extracted pectin. These results indicate that extraction yield of pumpkin pectin would be improved by microwave extraction and different pectin structure and properties can be obtained compared to acid extraction. Pumpkin is a promising alternative source for pectin material. Pumpkin pectin has a unique chemical structure and physical properties, presumably providing different functional properties compared to conventional commercial pectin sources. Depending on the conditions to produce pumpkin pectin, diverse molecular structures can be obtained and utilized in various food applications. © 2012 Institute of Food Technologists®

Modified Lipid Extraction Methods for Deep Subsurface Shale

PubMed Central

Akondi, Rawlings N.; Trexler, Ryan V.; Pfiffner, Susan M.; Mouser, Paula J.; Sharma, Shikha

2017-01-01

Growing interest in the utilization of black shales for hydrocarbon development and environmental applications has spurred investigations of microbial functional diversity in the deep subsurface shale ecosystem. Lipid biomarker analyses including phospholipid fatty acids (PLFAs) and diglyceride fatty acids (DGFAs) represent sensitive tools for estimating biomass and characterizing the diversity of microbial communities. However, complex shale matrix properties create immense challenges for microbial lipid extraction procedures. Here, we test three different lipid extraction methods: modified Bligh and Dyer (mBD), Folch (FOL), and microwave assisted extraction (MAE), to examine their ability in the recovery and reproducibility of lipid biomarkers in deeply buried shales. The lipid biomarkers were analyzed as fatty acid methyl esters (FAMEs) with the GC-MS, and the average PL-FAME yield ranged from 67 to 400 pmol/g, while the average DG-FAME yield ranged from 600 to 3,000 pmol/g. The biomarker yields in the intact phospholipid Bligh and Dyer treatment (mBD + Phos + POPC), the Folch, the Bligh and Dyer citrate buffer (mBD-Cit), and the MAE treatments were all relatively higher and statistically similar compared to the other extraction treatments for both PLFAs and DGFAs. The biomarker yields were however highly variable within replicates for most extraction treatments, although the mBD + Phos + POPC treatment had relatively better reproducibility in the consistent fatty acid profiles. This variability across treatments which is associated with the highly complex nature of deeply buried shale matrix, further necessitates customized methodological developments for the improvement of lipid biomarker recovery. PMID:28790998

Method for extracting lanthanides and actinides from acid solutions by modification of Purex solvent

DOEpatents

Horwitz, E.P.; Kalina, D.G.

1986-03-04

A process is described for the recovery of actinide and lanthanide values from aqueous solutions with an extraction solution containing an organic extractant having the formula as shown in a diagram where [phi] is phenyl, R[sup 1] is a straight or branched alkyl or alkoxyalkyl containing from 6 to 12 carbon atoms and R[sup 2] is an alkyl containing from 3 to 6 carbon atoms and phase modifiers in a water-immiscible hydrocarbon diluent. The addition of the extractant to the Purex process extractant, tri-n-butylphosphate in normal paraffin hydrocarbon diluent, will permit the extraction of multivalent lanthanide and actinide values from 0.1 to 12.0 molar acid solutions. 6 figs.

PROCESS FOR PRODUCING ALKYL ORTHOPHOSPHORIC ACID EXTRACTANTS

DOEpatents

Grinstead, R.R.

1962-01-23

A process is given for producing superior alkyl orthophosphoric acid extractants for use in solvent extraction methods to recover and purify various metals such as uranium and vanadium. The process comprises slurrying P/sub 2/O/ sub 5/ in a solvent diluent such as kerosene, benzene, isopropyl ether, and the like. An alipbatic alcohol having from nine to seventeen carbon atoms, and w- hcrein ihc OH group is situated inward of the terminal carbon atoms, is added to the slurry while the reaction temperature is mainiained below 60 deg C. The alcohol is added in the mole ratio of about 2 to l, alcohol to P/sub 2/O/sub 5/. A pyrophosphate reaotion product is formed in the slurry-alcohol mixture. Subsequently, the pyrophosphate reaction product is hydrolyzed with dilute mineral acid to produce the desired alkyl orthophosphoric aeid extractant. The extraetant may then be separated and utilized in metal-recovery, solvent- extraction processes. (AEC)

Homogenization versus homogenization-free method to measure muscle glycogen fractions.

PubMed

Mojibi, N; Rasouli, M

2016-12-01

The glycogen is extracted from animal tissues with or without homogenization using cold perchloric acid. Three methods were compared for determination of glycogen in rat muscle at different physiological states. Two groups of five rats were kept at rest or 45 minutes muscular activity. The glycogen fractions were extracted and measured by using three methods. The data of homogenization method shows that total glycogen decreased following 45 min physical activity and the change occurred entirely in acid soluble glycogen (ASG), while AIG did not change significantly. Similar results were obtained by using "total-glycogen-fractionation methods". The findings of "homogenization-free method" indicate that the acid insoluble fraction (AIG) was the main portion of muscle glycogen and the majority of changes occurred in AIG fraction. The results of "homogenization method" are identical with "total glycogen fractionation", but differ with "homogenization-free" protocol. The ASG fraction is the major portion of muscle glycogen and is more metabolically active form.

Application of an online post-column derivatization HPLC-DPPH assay to detect compounds responsible for antioxidant activity in Sonchus oleraceus L. leaf extracts.

PubMed

Ou, Zong-Quan; Schmierer, David M; Rades, Thomas; Larsen, Lesley; McDowell, Arlene

2013-02-01

To use an online assay to identify key antioxidants in Sonchus oleraceus leaf extracts and to investigate the effect of leaf position and extraction conditions on antioxidant concentration and activity. Separation of phytochemicals and simultaneous assessment of antioxidant activity were performed online using HPLC and post-column reaction with a free-radical reagent (2, 2-diphenylpicrylhydrazyl, DPPH). Active compounds were identified using nuclear magnetic resonance spectroscopy and mass spectrometry. We applied the online HPLC-DPPH radical assay to evaluate antioxidants in leaves from different positions on the plant and to assess the effect of pre-treatment of leaves with liquid N(2) before grinding, extraction time, extraction temperature and method of concentrating extracts. Key antioxidants identified in S. oleraceus leaf extracts were caftaric acid, chlorogenic acid and chicoric acid. Middle leaves contained the highest total amount of the three key antioxidant compounds, consisting mainly of chicoric acid. Pre-treatment with liquid N(2), increasing the extraction temperature and time and freeze-drying the extract did not enhance the yield of the key antioxidants. The online HPLC-DPPH radical assay was validated as a useful screening tool for investigating individual antioxidants in leaf extracts. Optimized extraction conditions were middle leaves pre-treated with liquid N(2), extraction at 25°C for 0.5 h and solvent removal by rotary evaporation. © 2012 The Authors. JPP © 2012. Royal Pharmaceutical Society.

Method of analysis at the U.S. Geological Survey California Water Science Center, Sacramento Laboratory - determination of haloacetic acid formation potential, method validation, and quality-control practices

USGS Publications Warehouse

Zazzi, Barbara C.; Crepeau, Kathryn L.; Fram, Miranda S.; Bergamaschi, Brian A.

2005-01-01

An analytical method for the determination of haloacetic acid formation potential of water samples has been developed by the U.S. Geological Survey California Water Science Center Sacramento Laboratory. The haloacetic acid formation potential is measured by dosing water samples with chlorine under specified conditions of pH, temperature, incubation time, darkness, and residual-free chlorine. The haloacetic acids formed are bromochloroacetic acid, bromodichloroacetic acid, dibromochloroacetic acid, dibromoacetic acid, dichloroacetic acid, monobromoacetic acid, monochloroacetic acid, tribromoacetic acid, and trichloroacetic acid. They are extracted, methylated, and then analyzed using a gas chromatograph equipped with an electron capture detector. Method validation experiments were performed to determine the method accuracy, precision, and detection limit for each of the compounds. Method detection limits for these nine haloacetic acids ranged from 0.11 to 0.45 microgram per liter. Quality-control practices include the use of blanks, quality-control samples, calibration verification standards, surrogate recovery, internal standard, matrix spikes, and duplicates.

Rapid LC-MS Determination of Acromelic Acids A and B, Toxic Constituents of the Mushroom Paralepistopsis acromelalga.

PubMed

Yoshioka, Naoki; Ouchi, Hitoshi; Kan, Toshiyuki; Yoshida, Masashi; Nomura, Motoyuki

2017-01-01

A rapid LC-MS method was developed for determination of acromelic acids A and B, which are toxic constituents of Paralepistopsis acromelalga (=Clitocybe acromelalga), in mushroom samples. Acromelic acids were extracted twice with 50% methanol and the extract was passed through a syringe filter, and then analyzed by LC-MS. The LC separation was performed on a multi-mode ODS column. The recoveries of acromelic acids A and B spiked into blank mushroom samples at 2.5 μg/g were 93 and 74%, respectively. This method was applied to the remaining mushroom sample from a food poisoning case. Acromelic acids A and B were detected at 2.0 and 1.4 μg/g, respectively, in the remaining sample. Another toxic constituent, which appeared to be clitidine, was also detected in the sample.

Optimization of a new method for extraction of cyanidin chloride and pelargonidin chloride anthocyanins with magnetic solid phase extraction and determination in fruit samples by HPLC with central composite design.

PubMed

Yari, Abdollah; Rashnoo, Saba

2017-11-01

Here, we are reporting a sensitive, simple and rapid method for the analysis of cyanidin chloride and pelargonidin chloride anthocyanins in cherry, sour cherry, pomegranate and barberry produced in Iran. The analytes were extracted with acetonitrile-hydrochloric acid (1% v/v) mixture under optimized pretreatment conditions. Clean-up of the extract from fruits was conducted by magnetic solid phase extraction using salicylic acid functionalized silica-coated magnetite nanoparticles (SCMNPs) as the adsorbent. The optimized conditions searched with central composite design. Working under optimum conditions specified as: SCMNPs modified with salicylic acid, sorbent contact time and sample 10min, mechanical stirring time 57.3min. HPLC with UV-detection was used for determination of the analytes. The limit of detection, LOD, obtained for the two anthocyanins were 0.02 and 0.03μgg -1 , respectively. The ranges of the spiked recoveries were 80.0-97.6 and 72.9-97.2%, with the relative standard deviations (RSD) of 2.1 and 2.5%, respectively. Copyright © 2017 Elsevier B.V. All rights reserved.

Improved sample extraction and clean-up for the GC-MS determination of BADGE and BFDGE in vegetable oil.

PubMed

Brede, C; Skjevrak, I; Herikstad, H; Anensen, E; Austvoll, R; Hemmingsen, T

2002-05-01

A straightforward method was established for the determination of migration contaminants in olive oil with a special focus on the two can-coating migration compounds bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE). The preferred sample preparation was a single liquid-liquid extraction of compounds from the oil into 20% (v/v) methanol in acetonitrile, followed by clean-up with solid-phase extraction on aminopropyl bonded to silica. This purification procedure selectively removed all free fatty acids from the extracts without removing phenolic compounds of interest. The solid-phase extraction columns were used many times by implementing a procedure of washing out the strongly retained fatty acids with 2% acetic acid in methanol. Gas chromatography coupled with full scan (m/z 33-700) electron ionization mass spectrometry was used for the determination of several model compounds in olive oil samples. BADGE and BFDGE could be determined in the 0.05-2 mg kg(-1) range in oil samples with a relative SD of <6% (six replicates). The method was used in an enforcement campaign for the Norwegian Food Control Authority to analyse vegetable oil samples from canned fish-in-oil.

Identification of Bioactivity, Volatile and Fatty Acid Profile in Supercritical Fluid Extracts of Mexican arnica.

PubMed

García-Pérez, J Saúl; Cuéllar-Bermúdez, Sara P; Arévalo-Gallegos, Alejandra; Rodríguez-Rodríguez, José; Iqbal, Hafiz M N; Parra-Saldivar, Roberto

2016-09-12

Supercritical fluid extraction (SFE) is a sustainable technique used for the extraction of lipophilic metabolites such as pigments and fatty acids. Arnica plant is considered a potential candidate material with high antioxidant and antimicrobial activities. Therefore, in this study, a locally available Heterotheca inuloides, also known as Mexican arnica, was analyzed for the extraction of high-value compounds. Based on different pressure (P), temperature (T), and co-solvent (CoS), four treatments (T) were prepared. A maximum 7.13% yield was recovered from T2 (T = 60 °C, P = 10 MPa, CoS = 8 g/min), followed by 6.69% from T4 (T = 60 °C, P = 30 MPa, CoS = 4 g/min). Some bioactive sesquiterpenoids such as 7-hydroxycadalene, caryophyllene and δ-cadinene were identified in the extracts by GC/MS. The fatty acid profile revealed that the main components were palmitic acid (C16:0), followed by linoleic acid (C18:2ω6c), α-linolenic acid (C18:3ω3) and stearic acid (C18:0) differing in percent yield per treatment. Antibacterial activities were determined by the agar diffusion method, indicating that all the treatments exerted strong antibacterial activity against S. aureus, C. albicans, and E. coli strains. The antioxidant capacity of the extracts was also measured by three in vitro assays, DPPH, TEAC and FRAP, using Trolox as a standard. Results showed high antioxidant capacity enabling pharmaceutical applications of Mexican arnica.

Identification of Bioactivity, Volatile and Fatty Acid Profile in Supercritical Fluid Extracts of Mexican arnica

PubMed Central

García-Pérez, J. Saúl; Cuéllar-Bermúdez, Sara P.; Arévalo-Gallegos, Alejandra; Rodríguez-Rodríguez, José; Iqbal, Hafiz M. N.; Parra-Saldivar, Roberto

2016-01-01

Supercritical fluid extraction (SFE) is a sustainable technique used for the extraction of lipophilic metabolites such as pigments and fatty acids. Arnica plant is considered a potential candidate material with high antioxidant and antimicrobial activities. Therefore, in this study, a locally available Heterotheca inuloides, also known as Mexican arnica, was analyzed for the extraction of high-value compounds. Based on different pressure (P), temperature (T), and co-solvent (CoS), four treatments (T) were prepared. A maximum 7.13% yield was recovered from T2 (T = 60 °C, P = 10 MPa, CoS = 8 g/min), followed by 6.69% from T4 (T = 60 °C, P = 30 MPa, CoS = 4 g/min). Some bioactive sesquiterpenoids such as 7-hydroxycadalene, caryophyllene and δ-cadinene were identified in the extracts by GC/MS. The fatty acid profile revealed that the main components were palmitic acid (C16:0), followed by linoleic acid (C18:2ω6c), α-linolenic acid (C18:3ω3) and stearic acid (C18:0) differing in percent yield per treatment. Antibacterial activities were determined by the agar diffusion method, indicating that all the treatments exerted strong antibacterial activity against S. aureus, C. albicans, and E. coli strains. The antioxidant capacity of the extracts was also measured by three in vitro assays, DPPH, TEAC and FRAP, using Trolox as a standard. Results showed high antioxidant capacity enabling pharmaceutical applications of Mexican arnica. PMID:27626416

A rapid quantitative determination of phenolic acids in Brassica oleracea by capillary zone electrophoresis.

PubMed

Lee, Iris S L; Boyce, Mary C; Breadmore, Michael C

2011-07-15

A simple and rapid capillary zone electrophoresis method to quantitatively determine the phenolic acid contents in brassica vegetables is described. Phenolic compounds were extracted from broccoli, broccolini, Brussels sprouts, cabbage and cauliflower and the main hydroxycinnamic acids (sinapic, ferulic, p-coumaric and caffeic acids) were isolated by solid phase extraction with C18 cartridges. Using an optimised method, the four analytes were separated in less than 7min in a 50μm×60cm capillary with a 15mM borate buffer (pH=9.13) and a separation voltage of 30kV at 30°C. A linear relationship was observed for the method (r=0.9997-0.9999) with detection limits ranging from 1.1 to 2.3mg/kg of vegetables for the analytes. This method demonstrated good reproducibility with coefficients of variation of less than 5% for peak area and less than 1% for migration time (n=7). The method was successfully applied to quantitatively determine the phenolic acid contents in a range of brassica vegetables and the results were in good agreement when compared to those from high performance liquid chromatography analysis. Crown Copyright © 2011. Published by Elsevier Ltd. All rights reserved.

Development and validation of an efficient ultrasound assisted extraction of phenolic compounds from flax (Linum usitatissimum L.) seeds.

PubMed

Corbin, Cyrielle; Fidel, Thibaud; Leclerc, Emilie A; Barakzoy, Esmatullah; Sagot, Nadine; Falguiéres, Annie; Renouard, Sullivan; Blondeau, Jean-Philippe; Ferroud, Clotilde; Doussot, Joël; Lainé, Eric; Hano, Christophe

2015-09-01

Flaxseed accumulates in its seedcoat a macromolecular complex composed of lignan (secoisolariciresinol diglucoside, SDG), flavonol (herbacetin diglucoside, HDG) and hydroxycinnamic acids (p-couramic, caffeic and ferulic acid glucosides). Their antioxidant and/or cancer chemopreventive properties support their interest in human health and therefore, the demand for their extraction. In the present study, ultrasound-assisted extraction (UAE) of flaxseed phenolic compounds was investigated. Scanning Electron Microscopy imaging and histochemical analysis revealed the deep alteration of the seedcoat ultrastructure and the release of the mucilage following ultrasound treatment. Therefore, this method was found to be very efficient for the reduction of mucilage entrapment of flaxseed phenolics. The optimal conditions for UAE phenolic compounds extraction from flaxseeds were found to be: water as solvent supplemented with 0.2N of sodium hydroxide for alkaline hydrolysis of the SDG-HMG complex, an extraction time of 60 min at a temperature of 25°C and an ultrasound frequency of 30 kHz. Under these optimized and validated conditions, highest yields of SDG, HDG and hydroxycinnamic acid glucosides were detected in comparison to other published methods. Therefore, the procedure presented herein is a valuable method for efficient extraction and quantification of the main flaxseed phenolics. Moreover, this UAE is of particular interest within the context of green chemistry in terms of reducing energy consumption and valuation of flaxseed cakes as by-products resulting from the production of flax oil. Copyright © 2015 Elsevier B.V. All rights reserved.

Extraction, composition and functional properties of pennycress (Thlaspi arvense L.) press cake protein

USDA-ARS?s Scientific Manuscript database

This study compared two methods for extracting the protein in pennycress (Thlaspi arvense L.) press cake and determined the composition and functional properties of the protein products. Proteins in pennycress press cake were extracted by using the conventional alkali solubilization-acid precipitati...

Solvent and extraction methods effects on the quality of eel (Anguilla bicolor) oil

NASA Astrophysics Data System (ADS)

Sasongko, H.; Efendi, N. R.; Budihardjo, A.; Farida, Y.; Amartiwi, T.; Rahmawati, A. A.; Wicaksono, A.; Sugiyarto

2017-01-01

Eel (Anguilla bicolor) is a general fish consumption in many countries, especially Japan, China, Germany, and France. Besides its vitamin rich, eel oil is also known to contain fatty acids that are necessary for pharmaceutical purposes and as food a supplement. This research was aimed to evaluate the quality of eel oil by different solvent and extraction methods. In this study, fresh eels were extracted using maceration and reflux methods.Chloroform was used as the solvent in the maceration while water used in the reflux method. The oil quality was examined based on the Official Methods of Analysis of the Association of Official Analytical Chemist (AOAC).The result showed that the yield of eel oil using maceration method was 5.44% ± 0.64 with a specific gravity of 0.915 g/mL, while reflux method obtained the yield of 5.33 % ± 0.84 and specific gravity of 0.8575 g/mL. The physicochemical parameters of oil quality used in this study were acid, peroxide, saponification, and iodine value. The maceration method obtained the acid value of 17.389 mgKOH/g, the peroxide value of 7.021meqO2/kg, the saponification value of 111.16mgKOH/g, and the iodine value of 65.14 WIJS. While the reflux method produced the acid value of 9.116 mgKOH/g, the peroxide value of 6.088 meqO2/kg, the saponification value of 70 mgKOH/g, and the iodine value of 87.74 WIJS.

Comparative study on anti-oxidant and anti-inflammatory activities of Caesalpinia crista and Centella asiatica leaf extracts

PubMed Central

Ramesh, B. N.; Girish, T. K.; Raghavendra, R. H.; Naidu, K. Akhilender; Rao, U. J. S. Prasada; Rao, K. S.

2014-01-01

Background: Amyloidosis, oxidative stress and inflammation have been strongly implicated in neurodegenerative disorders like Alzheimer's disease. Traditionally, Caesalpinia crista and Centella asiatica leaf extracts are used to treat brain related diseases in India. C. crista is used as a mental relaxant drink as well as to treat inflammatory diseases, whereas C. asiatica is reported to be used to enhance memory and to treat dementia. Objective: The present study is aimed to understand the anti-oxidant and anti-inflammatory potential of C. asiatica and C. crista leaf extracts. Materials and Methods: Phenolic acid composition of the aqueous extracts of C. crista and C. asiatica were separated on a reverse phase C18 column (4.6 x 250 mm) using HPLC system. Antioxidant properties of the leaf extracts were determined by 1,1-diphenyl-2-picrylhydrazyl (DPPH) radical scavenging assay and the reducing potential assay. The anti-inflammatory activities of aqueous extracts of C. crista and C. asiatica were studied using 5-lipoxygenase assay. Polymorphonuclear leukocytes (PMNLs) were isolated from blood by Ficoll-Histopaque density gradient followed by hypotonic lysis of erythrocytes. Results: Gallic, protocatechuic, gentisic, chlorogenic, caffeic, p-coumaric and ferulic acids were the phenolic acids identified in C. crista and C. asiatica leaf aqueous extracts. However, gallic acid and ferulic acid contents were much higher in C. crista compared to C. asiatica. Leaf extracts of C. asiatica and C. crista exhibited antioxidant properties and inhibited 5-lipoxygenase (anti-inflammatory) in a dose dependent manner. However, leaf extracts of C. crista had better antioxidant and anti-inflammatory activity compared to that of C. asiatica. The better activity of C. crista is attributed to high gallic acid and ferulic acid compared to C. asiatica. Conclusions: Thus, the leaf extract of C. crista can be a potential therapeutic role for Alzheimer's disease. PMID:24741275

Identification of Phenolic Compounds and Evaluation of Antioxidant and Antimicrobial Properties of Euphorbia Tirucalli L.

PubMed Central

de Araújo, Keline Medeiros; de Lima, Alessandro; Silva, Jurandy do N.; Rodrigues, Larissa L.; Amorim, Adriany G. N.; Quelemes, Patrick V.; dos Santos, Raimunda C.; Rocha, Jefferson A.; de Andrades, Éryka O.; Leite, José Roberto S. A.; Mancini-Filho, Jorge; da Trindade, Reginaldo Almeida

2014-01-01

Bioactive compounds extracted from natural sources can benefit human health. The aim of this work was to determine total phenolic content and antioxidant activity in extracts of Euphorbia tirucalli L. followed by identification and quantification of the phenolic compounds, as well as their antibacterial activities. Antioxidant activities were determined by DPPH and ABTS•+ assay. Identification of phenolic compounds was performed using high-performance liquid chromatography (HPLC), and antimicrobial activities were verified by agar dilution methods and MIC values. Total phenolic content ranged from 7.73 to 30.54 mg/100 g gallic acid equivalent. Extracts from dry plants showed higher antioxidant activities than those from fresh ones. The DPPH EC50 values were approximately 12.15 μg/mL and 16.59 μg/mL, respectively. Antioxidant activity measured by the ABTS method yielded values higher than 718.99 μM trolox/g for dry plants, while by the Rancimat® system yielded protection factors exceeding 1 for all extracts, comparable to synthetic BHT. Ferulic acid was the principal phenolic compound identified and quantified through HPLC-UV in all extracts. The extracts proved effective inhibitory potential for Staphylococcus epidermidis and Staphylococcus aureus. These results showed that extracts of Euphorbia tirucalli L. have excellent antioxidant capacity and moderate antimicrobial activity. These can be attributed to the high concentration of ferulic acid. PMID:26784670

Simple and rapid analytical method for detection of amino acids in blood using blood spot on filter paper, fast-GC/MS and isotope dilution technique.

PubMed

Kawana, Shuichi; Nakagawa, Katsuhiro; Hasegawa, Yuki; Yamaguchi, Seiji

2010-11-15

A simple and rapid method for quantitative analysis of amino acids, including valine (Val), leucine (Leu), isoleucine (Ile), methionine (Met) and phenylalanine (Phe), in whole blood has been developed using GC/MS. In this method, whole blood was collected using a filter paper technique, and a 1/8 in. blood spot punch was used for sample preparation. Amino acids were extracted from the sample, and the extracts were purified using cation-exchange resins. The isotope dilution method using ²H₈-Val, ²H₃-Leu, ²H₃-Met and ²H₅-Phe as internal standards was applied. Following propyl chloroformate derivatization, the derivatives were analyzed using fast-GC/MS. The extraction recoveries using these techniques ranged from 69.8% to 87.9%, and analysis time for each sample was approximately 26 min. Calibration curves at concentrations from 0.0 to 1666.7 μmol/l for Val, Leu, Ile and Phe and from 0.0 to 333.3 μmol/l for Met showed good linearity with regression coefficients=1. The method detection limits for Val, Leu, Ile, Met and Phe were 24.2, 16.7, 8.7, 1.5 and 12.9 μmol/l, respectively. This method was applied to blood spot samples obtained from patients with phenylketonuria (PKU), maple syrup urine disease (MSUD), hypermethionine and neonatal intrahepatic cholestasis caused by citrin deficiency (NICCD), and the analysis results showed that the concentrations of amino acids that characterize these diseases were increased. These results indicate that this method provides a simple and rapid procedure for precise determination of amino acids in whole blood. Copyright © 2010 Elsevier B.V. All rights reserved.

Validation of internal controls for extraction and amplification of nucleic acids from enteric viruses in water samples.

PubMed

Hata, Akihiko; Katayama, Hiroyuki; Kitajima, Masaaki; Visvanathan, Chettiyappan; Nol, Chea; Furumai, Hiroaki

2011-07-01

Inhibitors that reduce viral nucleic acid extraction efficiency and interfere with cDNA synthesis and/or polymerase activity affect the molecular detection of viruses in aquatic environments. To overcome these significant problems, we developed a methodology for assessing nucleic acid yields and DNA amplification efficiencies for environmental water samples. This involved adding particles of adenovirus type 5 and murine norovirus and newly developed primer-sharing controls, which are amplified with the same primer pairs and result in the same amplicon sizes as the targets, to these samples. We found that nucleic acid loss during the extraction process, rather than reverse transcription-PCR (RT-PCR) inhibition, more significantly attributed to underestimation of the presence of viral genomes in the environmental water samples tested in this study. Our success rate for satisfactorily amplifying viral RNAs and DNAs by RT-PCR was higher than that for obtaining adequate nucleic acid preparations. We found that inhibitory properties were greatest when we used larger sample volumes. A magnetic silica bead-based RNA extraction method effectively removed inhibitors that interfere with viral nucleic acid extraction and RT-PCR. To our knowledge, this is the first study to assess the inhibitory properties of environmental water samples by using both control virus particles and primer-sharing controls.

Determination of trigonelline, nicotinic acid, and caffeine in Yunnan Arabica coffee by microwave-assisted extraction and HPLC with two columns in series.

PubMed

Liu, Hongcheng; Shao, Jinliang; Li, Qiwan; Li, Yangang; Yan, Hong Mei; He, Lizhong

2012-01-01

A simple, rapid method was developed for simultaneous extraction of trigonelline, nicotinic acid, and caffeine from coffee, and separation by two chromatographic columns in series. The trigonelline, nicotinic acid, and caffeine were extracted with microwave-assisted extraction (MAE). The optimal conditions selected were 3 min, 200 psi, and 120 degrees C. The chromatographic separation was performed with two columns in series, polyaromatic hydrocarbon C18 (250 x 4.6 mm id, 5 microm particle size) and Bondapak NH2 (300 x 3.9 mm id, 5 microm particle size). Isocratic elution was with 0.02 M phosphoric acid-methanol (70 + 30, v/v) mobile phase at a flow rate of 0.8 mL/min. Good recoveries and RSD values were found for all analytes in the matrix. The LOD of the three compounds was 0.02 mg/L, and the LOQ was 0.005% in the matrix. The concentrations of trigonelline, nicotinic acid, and caffeine in instant coffee, roasted coffee, and raw coffee (Yunnan Arabica coffee) were assessed by MAE and hot water extraction; the correlation coefficients between concentrations of the three compounds obtained were close to 1.

Molecular characteristics of humic acids isolated from vermicomposts and their relationship to bioactivity.

PubMed

Martinez-Balmori, Dariellys; Spaccini, Riccardo; Aguiar, Natália Oliveira; Novotny, Etelvino Henrique; Olivares, Fábio Lopes; Canellas, Luciano Pasqualoto

2014-11-26

Vermitechnology is an effective composting method, which transforms biomass into nutrient-rich organic fertilizer. Mature vermicompost is a renewable organic product containing humic substances with high biological activity. The aim of this study was to assess the chemical characteristics and the bioactivity of humic acids isolated from different vermicomposts produced with either cattle manure, sugar cane bagasse, sunflower cake from seed oil extraction, or filter cake from a sugar cane factory. More than 200 different molecules were found, and it was possible to identify chemical markers on humic acids according to the nature of the organic source. The large hydrophobic character of humic extracts and the preservation of altered lignin derivatives confer to humic acids the ability to induce lateral root emergence in maize seedlings. Humic acid-like substances extracted from plant biomass residues represent an additional valuable product of vermicomposting that can be used as a plant growth promoter.

Method of extracting iodine from liquid mixtures of iodine, water and hydrogen iodide

DOEpatents

Mysels, Karol J.

1979-01-01

The components of a liquid mixture consisting essentially of HI, water and at least about 50 w/o iodine are separated in a countercurrent extraction zone by treating with phosphoric acid containing at least about 90 w/o H.sub.3 PO.sub.4. The bottom stream from the extraction zone is substantially completely molten iodine, and the overhead stream contains water, HI, H.sub.3 PO.sub.4 and a small fraction of the amount of original iodine. When the water and HI are present in near-azeotropic proportions, there is particular advantage in feeding the overhead stream to an extractive distillation zone wherein it is treated with additional concentrated phosphoric acid to create an anhydrous HI vapor stream and bottoms which contain at least about 85 w/o H.sub.3 PO.sub.4. Concentration of these bottoms provides phosphoric acid infeed for both the countercurrent extraction zone and for the extractive distillation zone.

Ultrasound assisted extraction of polyphenols and their distribution in whole mung bean, hull and cotyledon.

PubMed

Singh, Barinderjit; Singh, Narpinder; Thakur, Sheetal; Kaur, Amritpal

2017-03-01

In this study, extraction of polyphenols using different solvents (acetone, ethanol, methanol and water) with ultrasound and conventional method from whole mung bean (WMB), hull and cotyledon was conducted. Total phenolic content (TPC), total flavonoids content (TFC), total antioxidant activities (TAA), ferric reducing power (FRP) and DPPH radical scavenging activity were determined. Ultrasound treated extracts exhibited higher TPC, TFC, TAA, FRP and DPPH in different mung bean fractions than CSE. Among the solvents, acetone showed better TPC, TFC, TAA, FRP and DPPH. Hull had significantly higher TPC, TFC, TAA, FRP and DPPH than WMB and cotyledon. Sinapic acid (SA) was the major polyphenol in different fractions. Acetone extract of hull showed high polyphenol content. SA, ferulic acid, catechin, p-coumaric acid, resveratrol, quercetin and luteolin were the major contributors to antioxidant activity of acetone extract. Mung bean hull contained the maximum polyphenols and acetone was observed to be the best extraction medium for polyphenols in combination with ultrasound.

Evaluation of different methods of protein extraction and identification of differentially expressed proteins upon ethylene-induced early-ripening in banana peels.

PubMed

Zhang, Li-Li; Feng, Ren-Jun; Zhang, Yin-Dong

2012-08-15

Banana peels (Musa spp.) are a good example of a plant tissue where protein extraction is challenging due to the abundance of interfering metabolites. Sample preparation is a critical step in proteomic research and is critical for good results. We sought to evaluate three methods of protein extraction: trichloroacetic acid (TCA)-acetone precipitation, phenol extraction, and TCA precipitation. We found that a modified phenol extraction protocol was the most optimal method. SDS-PAGE and two-dimensional gel electrophoresis (2-DE) demonstrated good protein separation and distinct spots of high quality protein. Approximately 300 and 550 protein spots were detected on 2-DE gels at pH values of 3-10 and 4-7, respectively. Several spots were excised from the 2-DE gels and identified by mass spectrometry. The protein spots identified were found to be involved in glycolysis, the tricarboxylic acid cycle, and the biosynthesis of ethylene. Several of the identified proteins may play important roles in banana ripening. Copyright © 2012 Society of Chemical Industry.

Development of a HPLC-UV method for the quantitative determination of four short-chain fatty acids and lactic acid produced by intestinal bacteria during in vitro fermentation.

PubMed

De Baere, S; Eeckhaut, V; Steppe, M; De Maesschalck, C; De Backer, P; Van Immerseel, F; Croubels, S

2013-06-01

A rapid and sensitive HPLC-UV method for the quantitative determination of four short-chain fatty acids (SCFAs) and lactic acid (LA) produced during in vitro fermentation is presented. Extraction of SCFAs from supernatants of bacterial cultures is aggravated due to their polarity and volatility. Detection can only be performed at a short, non-selective UV wavelength (210nm), due to the lack of any significant chromophore. Therefore special attention was paid to the optimization of the sample preparation procedure and the HPLC-UV conditions. The final extraction procedure consisted of a liquid-liquid back extraction using diethylether. Prior to HPLC-UV analysis the samples were acidified (pH<2) in order to improve retention of the SCFA's and LA on the Hypersil Gold aQ column. Matrix-matched calibration graphs were prepared for all analytes of interest (range 0.5-50mM) and correlation and goodness-of-fit coefficients were between 0.9951-0.9993 and 3.88-8.27%, respectively. Limits of detection and quantification ranged from 0.13 to 0.33mM and 0.5 to 1.0mM, respectively. The results for the within-day and between-day precision and accuracy fell within the ranges specified. The reported validated method has been successfully used for the in vitro screening of supernatants of bacterial cultures for the presence of butyric acid, aiming to select for butyric acid-producing bacteria. In addition, the method has been used to determine the production pattern of selected fatty acids by bacterial species isolated from human feces and chicken caeca. Copyright © 2013 Elsevier B.V. All rights reserved.

Literature mining of protein-residue associations with graph rules learned through distant supervision.

PubMed

Ravikumar, Ke; Liu, Haibin; Cohn, Judith D; Wall, Michael E; Verspoor, Karin

2012-10-05

We propose a method for automatic extraction of protein-specific residue mentions from the biomedical literature. The method searches text for mentions of amino acids at specific sequence positions and attempts to correctly associate each mention with a protein also named in the text. The methods presented in this work will enable improved protein functional site extraction from articles, ultimately supporting protein function prediction. Our method made use of linguistic patterns for identifying the amino acid residue mentions in text. Further, we applied an automated graph-based method to learn syntactic patterns corresponding to protein-residue pairs mentioned in the text. We finally present an approach to automated construction of relevant training and test data using the distant supervision model. The performance of the method was assessed by extracting protein-residue relations from a new automatically generated test set of sentences containing high confidence examples found using distant supervision. It achieved a F-measure of 0.84 on automatically created silver corpus and 0.79 on a manually annotated gold data set for this task, outperforming previous methods. The primary contributions of this work are to (1) demonstrate the effectiveness of distant supervision for automatic creation of training data for protein-residue relation extraction, substantially reducing the effort and time involved in manual annotation of a data set and (2) show that the graph-based relation extraction approach we used generalizes well to the problem of protein-residue association extraction. This work paves the way towards effective extraction of protein functional residues from the literature.

Development of fast and robust multiresidual LC-MS/MS method for determination of pharmaceuticals in soils.

PubMed

Golovko, Oksana; Koba, Olga; Kodesova, Radka; Fedorova, Ganna; Kumar, Vimal; Grabic, Roman

2016-07-01

The aim of this study was to develop a simple extraction procedure and a multiresidual liquid chromatography-tandem mass spectrometry method for determination of a wide range of pharmaceuticals from various soil types. An extraction procedure for 91 pharmaceuticals from 13 soil types, followed by liquid chromatography-tandem mass spectrometry analysis, was optimized. The extraction efficiencies of three solvent mixtures for ultrasonic extraction were evaluated for 91 pharmaceuticals. The best results were obtained using acetonitrile/water (1/1 v/v with 0.1 % formic acid) followed by acetonitrile/2-propanol/water (3/3/4 v/v/v with 0.1 % formic acid) for extracting 63 pharmaceuticals. The method was validated at three fortification levels (10, 100, and 1000 ng/g) in all types of representative soils; recovery of 44 pharmaceuticals ranged between 55 and 135 % across all tested soils. The method was applied to analyze actual environmental samples of sediments, soils, and sludge, and 24 pharmaceuticals were found above limit of quantification with concentrations ranging between 0.83 ng/g (fexofenadine) and 223 ng/g (citalopram).

Method for rapid screening analysis of Sr-90 in edible plant samples collected near Fukushima, Japan.

PubMed

Amano, Hikaru; Sakamoto, Hideaki; Shiga, Norikatsu; Suzuki, Kaori

2016-06-01

A screening method for measuring (90)Sr in edible plant samples by focusing on (90)Y in equilibrium with (90)Sr is reported. (90)Y was extracted from samples with acid, co-precipitated with iron hydroxide, and precipitated with oxalic acid. The dissolved oxalate precipitate was loaded on an extraction chromatography resin, and the (90)Y-enriched eluate was analyzed by Cherenkov counting with a TDCR liquid scintillation counter. (90)Sr ((90)Y) concentration was determined in plant samples collected near the damaged Fukushima Daiichi Nuclear Power Plants with this method. Copyright © 2016 Elsevier Ltd. All rights reserved.

Development and application of an in-cell cleanup pressurized liquid extraction with ultra-high-performance liquid chromatography-tandem mass spectrometry to detect prohibited antiviral agents sensitively in livestock and poultry feces.

PubMed

Wu, Huizhen; Wang, Jianmei; Yang, Hua; Li, Guoqin; Zeng, Yinhuan; Xia, Wei; Li, Zuguang; Qian, Mingrong

2017-03-10

An in-cell cleanup pressurized liquid extraction was developed to analyze prohibited antiviral agents in livestock and poultry feces. Extraction and cleanup were integrated into one step. The extraction was performed using methanol-acetonitrile (1:1, v/v) with 0.5% glacial acetic acid at 90°C, and 0.75g of PSA was used as the adsorbent during the extraction procedure. Under optimal conditions, the average recoveries for 11 antiviral drugs were 71.5-112.5% at three spiked levels (20, 40, and 100μgkg -1 ). The detection limits and detection quantitations of the analysis method for the eleven antiviral drugs were 0.6-1.4 and 1.4-4.7μgkg -1 , respectively. Finally, the method was applied to analyze amantadine, oseltamivir and its metabolites oseltamivir acid in duck feces based on an experiment of an oral dose of two antiviral drugs in duck. The amantadine, oseltamivir and oseltamivir acid can be detected in feces within approximately four weeks after amantadine and oseltamivir were orally administered. The results indicate that the residue analysis in feces is a noninvasive method to monitor inhibited antiviral agents efficiently in livestock and poultry breeding. Copyright © 2017. Published by Elsevier B.V.

[A thin-layer chromatography method for determining the styrene metabolites mandelic and phenylglyoxylic acid in urine].

PubMed

Gartzke, J; Burck, D

1989-06-01

A thin-layer chromatographic method is described for the determination of mandelic and phenyglyoxillic acid on silicagel (Silufol UV 254) after extraction from urine of styrene exposed workers. The quantitative determination was performed after eluting the spots. Phenylglyoxilic acid was measured at 255 nm and mandelic acid by derivative spectroscopically estimation of the .CH(OH).COOH -chromophore at 217 nm or by a three-wavelength mode, respectively. The recovery in urine was 80-104% for phenylglyoxilic acid and 99-105% for mandelic acid.

Comparison of methods to determine selenium species in saturation extracts of soils from the western San Joaquin Valley, California

USGS Publications Warehouse

Fio, John L.; Fujii, Roger

1988-01-01

Undigested organic matter in some of the extracts inhibited selenium detection when using the digestion and Sep-Pac C18 methods, but the interference was removed by using the XAD-8 method. Combining XAD-8 resin and activated charcoal was an unacceptable method, because the activated charcoal removed selenite and selenate. Ninety-eight percent of the selenium in the extracts was selenate and about 100 percent of the isolated organic selenium was associated with the humic acid fraction of dissolved-organic matter.

Phytochemical Composition and Antioxidant Activities of Dianthus Thunbergii Hooper and Hypoxis Argentea Harv Ex Baker: Plants Used for the Management of Diabetes Mellitus in Eastern Cape, South Africa

PubMed Central

Akinrinde, Akinleye Stephen; Afolayan, Anthony Jide; Bradley, Graeme

2018-01-01

Background: Inhabitants of the Eastern Cape Province of South Africa use the roots of Dianthus thunbergii and corms of Hypoxis argentea to treat diabetes mellitus and other ailments. Objective: The objective of this study was to analyze the phytochemical composition and antioxidant activities of the aqueous and ethanol extracts of the roots and corms of two plants. Materials and Methods: Total phenolics, flavonoids, flavonols, proanthocyanidins, tannins, and alkaloids were determined by standard methods. The scavenging activities of the extracts against 1,1 diphenyl-2-picrylhydrazyl (DPPH), 2'-azino-bis (3-ethylbenthiazoline-6-sulfonic acid (ABTS), nitric oxide (NO), hydrogen peroxide (H2O2), and their ferric-reducing antioxidant potentials (FRAPs) were measured. Results: The ethanol extract of H. argentea had the highest content of phenolics (66.71 ± 2.71 mg gallic acid equivalent/g) and tannins (1.18 ± 0.07 mg TAE/g), while the ethanol extract of D. thunbergii gave higher contents of flavonoids and proanthocyanidins (62.21 ± 1.75 mg Qe/g and 432.62 ± 2.43 mg Ca/g, respectively). Flavonols were the most predominant in the aqueous extract of H. argentea (25.51 ± 1.92 mg Qe/g). We observed a concentration-dependent response in the ABTS- and H2O2-scavenging activities and FRAP values of the extracts and standards (Vitamin C, butylated hydroxytoluene, and rutin). The ethanol extracts of both plants generally demonstrated better antioxidant activities against H2O2, NO, and ABTS while also possessing better reducing power than the aqueous extracts. The aqueous extract of D. thunbergii, however, showed the best DPPH scavenging activity. Conclusion: The higher content of phytochemicals and antioxidant capacity obtained for the ethanol extracts of D. thunbergii and H. argentea may prove to be valuable information in selecting suitable extraction solvents for the medicinal applications of both plants. SUMMARY Ethanol extracts of Hypoxis argentea had the highest levels of phenolics and tanninsEthanol extracts of Dianthus thunbergii had the highest levels of flavonoids and proanthocyanidinsEthanol extracts of both plants possess better antioxidant activityagainst hydrogen peroxide, nitric oxide, and ABTS as well as higher reducingpower than the aqueous extractsAqueous extract of Dianthus thunbergii had the highest free radical scavenging activity as measured with DPPH. Abbreviations used: ABTS: 2'-azino-bis (3-ethylbenthiazoline-6-sulfonic acid); BHT: Butylated hydroxytoluene; DPPH: 1,1 diphenyl-2-picrylhydrazyl; DTA: Dianthus thunbergii aqueous extract (16.6%); DTE: Dianthus thunbergii ethanol extract (2.4%); Fe3+-TPTZ: Ferric tripyridyltriazine; FRAP: Ferric-reducing antioxidant potentials; GAE: Gallic acid equivalent; HAA: Hypoxis argentea aqueous extract (3.2%); HAE: Hypoxis argentea ethanol extract (1.8%); Qe: Quercetin equivalence; ROS: Reactive oxygen species; TBA: Thiobarbituric acid;TCA: Trichloroacetic acid. PMID:29720831

Metabolite extraction from adherently growing mammalian cells for metabolomics studies: optimization of harvesting and extraction protocols.

PubMed

Dettmer, Katja; Nürnberger, Nadine; Kaspar, Hannelore; Gruber, Michael A; Almstetter, Martin F; Oefner, Peter J

2011-01-01

Trypsin/ethylenediaminetetraacetic acid (EDTA) treatment and cell scraping in a buffer solution were compared for harvesting adherently growing mammalian SW480 cells for metabolomics studies. In addition, direct scraping with a solvent was tested. Trypsinated and scraped cell pellets were extracted using seven different extraction protocols including pure methanol, methanol/water, pure acetone, acetone/water, methanol/chloroform/water, methanol/isopropanol/water, and acid-base methanol. The extracts were analyzed by GC-MS after methoximation/silylation and derivatization with propyl chloroformate, respectively. The metabolic fingerprints were compared and 25 selected metabolites including amino acids and intermediates of energy metabolism were quantitatively determined. Moreover, the influence of freeze/thaw cycles, ultrasonication and homogenization using ceramic beads on extraction yield was tested. Pure acetone yielded the lowest extraction efficiency while methanol, methanol/water, methanol/isopropanol/water, and acid-base methanol recovered similar metabolite amounts with good reproducibility. Based on overall performance, methanol/water was chosen as a suitable extraction solvent. Repeated freeze/thaw cycles, ultrasonication and homogenization did not improve overall metabolite yield of the methanol/water extraction. Trypsin/EDTA treatment caused substantial metabolite leakage proving it inadequate for metabolomics studies. Gentle scraping of the cells in a buffer solution and subsequent extraction with methanol/water resulted on average in a sevenfold lower recovery of quantified metabolites compared with direct scraping using methanol/water, making the latter one the method of choice to harvest and extract metabolites from adherently growing mammalian SW480 cells.

Graphene/dodecanol floating solidification microextraction for the preconcentration of trace levels of cinnamic acid derivatives in traditional Chinese medicines.

PubMed

Hu, Shuang; Yang, Xiao; Xue, Jiao; Chen, Xuan; Bai, Xiao-Hong; Yu, Zhi-Hui

2017-07-01

A novel graphene/dodecanol floating solidification microextraction followed by HPLC with diode-array detection has been developed to extract trace levels of four cinnamic acid derivatives in traditional Chinese medicines. Several parameters affecting the performance were investigated and optimized. Also, possible microextraction mechanism was analyzed and discussed. Under the optimum conditions (amount of graphene in dodecanol: 0.25 mg/mL; volume of extraction phase: 70 μL; pH of sample phase: 3; extraction time: 30   min; stirring rate: 1000 rpm; salt amount: 26.5% NaCl; volume of sample phase: 10 mL, and without dispersant addition), the enrichment factors of four cinnamic acid derivatives ranged from 26 to 112, the linear ranges were 1.0 × 10 -2 -10.0 μg/mL for caffeic acid, 1.3 × 10 -3 -1.9 μg/mL for p-hydroxycinnamic acid, 2.8 × 10 -3 -4.1 μg/mL for ferulic acid, and 2.7 × 10 -3 -4.1 μg/mL for cinnamic acid, with r 2 ≥ 0.9993. The detection limits were found to be in the range of 0.1-1.0 ng/mL, and satisfactory recoveries (92.5-111.2%) and precisions (RSDs 1.1-9.5%) were also achieved. The results showed that the approach is simple, effective and sensitive for the preconcentration and determination of trace levels of cinnamic acid derivatives in Chinese medicines. The proposed method was compared with conventional dodecanol floating solidification microextraction and other extraction methods. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

[Effect of enzymolysis after acid and alkali pretreatment on extraction of tanshinones from Salviae Miltiorrhizae Radix et Rhizoma residues].

PubMed

Dai, Xin-Xin; Shen, Fei; Su, Shu-Lan; Zhang, Sen; Guo, Sheng; Jiang, Shu; Qian, Da-Wei; Duan, Jin-Ao

2016-09-01

Salviae Miltiorrhizae Radix et Rhizoma residues were pre-treated with acid and alkali, degraded by using cellulose, and the effects of different processing methods on the extraction rate of tanshinones were compared to provide scientific basis for development and utilization of tanshinones from Salviae Miltiorrhizae Radix et Rhizoma residues. The results showed that in the Salviae Miltiorrhizae Radix et Rhizoma residues without pre-treatment, enzymatic hydrolysis time of 4.5 d could make most of the cellulose degraded when the concentration of substrate enzyme concentration was 6 U•mL-1, and the highest glucose concentration was 59.74 mg•g⁻¹. It was found that the best effect was achieved after alkali pre-treatment-cellulose C degradation among the different pre-treatment methods, and the glucose content reached 119.50 mg•g⁻¹, followed by the same concentration of acid pre-treatment-cellulose C degradation. The extraction amount of tanshinone ⅡA was increased by 82.54% after enzyme degradation, with a mass fraction of 2.451 mg•g⁻¹; extraction amount of tanshinone I was increased by 81.82% after enzyme degradation, with a mass fraction of 2.373 mg•g⁻¹; extraction amount of cryptotanshinone was increased by 64.4% after enzyme degradation, with a mass fraction of 1.080 mg•g⁻¹; extraction amount of dihydrotanshinone I was increased by 61.3% after enzyme degradation, with a mass fraction of 0.601 2 mg•g⁻¹. Acid and alkali pre-treatment combined with cellulose degradation could effectively improve the extraction rate of tanshinones from Salviae Miltiorrhizae Radix et Rhizoma residues. This method is operable and practical, and it is beneficial for improving the utilization efficiency of tanshinones (resource based chemicals) from Salviae Miltiorrhizae Radix et Rhizoma residues. Copyright© by the Chinese Pharmaceutical Association.

A Method for Extracting Pigments from Squid Doryteuthis pealeii.

PubMed

DiBona, Christopher W; Williams, Thomas L; Dinneen, Sean R; Jones Labadie, Stephanie F; Deravi, Leila F

2016-11-09

Cephalopods can undergo rapid and adaptive changes in dermal coloration for sensing, communication, defense, and reproduction purposes. These capabilities are supported in part by the areal expansion and retraction of pigmented organs known as chromatophores. While it is known that the chromatophores contain a tethered network of pigmented granules, their structure-function properties have not been fully detailed. We describe a method for isolating the nanostructured granules in squid Doryteuthis pealeii chromatophores and demonstrate how their associated pigments can be extracted in acidic solvents. To accomplish this, the chromatophore containing dermal layer is first manually isolated using a superficial dissection, and the pigment granules are removed using sonication, centrifugation, and washing cycles. Pigments confined within the purified granules are then extracted via acidic methanol solutions, leaving nanostructures with smaller diameters that are void of visible color. This extraction procedure produces a 58% yield of soluble pigments isolated from granules. Using this method, the composition of the chromatophore pigments can be determined and used to provide insight into the mechanism of adaptive coloration in cephalopods.

Filtration Isolation of Nucleic Acids: A Simple and Rapid DNA Extraction Method.

PubMed

McFall, Sally M; Neto, Mário F; Reed, Jennifer L; Wagner, Robin L

2016-08-06

FINA, filtration isolation of nucleic acids, is a novel extraction method which utilizes vertical filtration via a separation membrane and absorbent pad to extract cellular DNA from whole blood in less than 2 min. The blood specimen is treated with detergent, mixed briefly and applied by pipet to the separation membrane. The lysate wicks into the blotting pad due to capillary action, capturing the genomic DNA on the surface of the separation membrane. The extracted DNA is retained on the membrane during a simple wash step wherein PCR inhibitors are wicked into the absorbent blotting pad. The membrane containing the entrapped DNA is then added to the PCR reaction without further purification. This simple method does not require laboratory equipment and can be easily implemented with inexpensive laboratory supplies. Here we describe a protocol for highly sensitive detection and quantitation of HIV-1 proviral DNA from 100 µl whole blood as a model for early infant diagnosis of HIV that could readily be adapted to other genetic targets.

Bioactive compounds and quality parameters of avocado oil obtained by different processes.

PubMed

Krumreich, Fernanda D; Borges, Caroline D; Mendonça, Carla Rosane B; Jansen-Alves, Cristina; Zambiazi, Rui C

2018-08-15

The objective of this study was to evaluate the quality of avocado oil whose pulp was processed through different drying and oil extraction methods. The physicochemical characteristics of avocados cv. Breda were determined after drying the pulp in an oven under ventilation (40 °C and 60 °C) and vacuum oven (60 °C), followed by the oil extracted by mechanical pressing or the Soxhlet method. From the approximately 72% pulp found in the avocado fruit, the 16% fraction is lipids. The quality indices evaluated in avocado oil showed better results when the pulp was dried at 60 °C under vacuum and oil extraction was done by the Soxhlet method with petroleum ether, whereas the bioactive compounds were better preserved when the avocado pulp was dried at 60 °C under ventilation and mechanical pressing was used for the oil extraction. Among the fatty acids found, oleic acid was the main. Copyright © 2018 Elsevier Ltd. All rights reserved.

Antibacterial, antioxidant and tyrosinase-inhibition activities of pomegranate fruit peel methanolic extract

PubMed Central

2012-01-01

Background This study evaluated, using in vitro assays, the antibacterial, antioxidant, and tyrosinase-inhibition activities of methanolic extracts from peels of seven commercially grown pomegranate cultivars. Methods Antibacterial activity was tested on Gram-positive (Bacillus subtilis and Staphylococcus aureus) and Gram-negative bacteria (Escherichia coli and Klebsiella pneumonia) using a microdilution method. Several potential antioxidant activities, including radical-scavenging ability (RSA), ferrous ion chelating (FIC) and ferric ion reducing antioxidant power (FRAP), were evaluated. Tyrosinase enzyme inhibition was investigated against monophenolase (tyrosine) and diphenolase (DOPA), with arbutin and kojic acid as positive controls. Furthermore, phenolic contents including total flavonoid content (TFC), gallotannin content (GTC) and total anthocyanin content (TAC) were determined using colourimetric methods. HPLC-ESI/MSn analysis of phenolic composition of methanolic extracts was also performed. Results Methanolic peel extracts showed strong broad-spectrum activity against Gram-positive and Gram-negative bacteria, with the minimum inhibitory concentrations (MIC) ranging from 0.2 to 0.78 mg/ml. At the highest concentration tested (1000 μg/ml), radical scavenging activities were significantly higher in Arakta (83.54%), Ganesh (83.56%), and Ruby (83.34%) cultivars (P< 0.05). Dose dependent FIC and FRAP activities were exhibited by all the peel extracts. All extracts also exhibited high inhibition (>50%) against monophenolase and diphenolase activities at the highest screening concentration. The most active peel extract was the Bhagwa cultivar against monophenolase and the Arakta cultivar against diphenolase with IC50 values of 3.66 μg/ml and 15.88 μg/ml, respectively. High amounts of phenolic compounds were found in peel extracts with the highest and lowest total phenolic contents of 295.5 (Ganesh) and 179.3 mg/g dry extract (Molla de Elche), respectively. Catechin, epicatechin, ellagic acid and gallic acid were found in all cultivars, of which ellagic acid was the most abundant comprising of more than 50% of total phenolic compounds detected in each cultivar. Conclusions The present study showed that the tested pomegranate peels exhibited strong antibacterial, antioxidant and tyrosinase-inhibition activities. These results suggest that pomegranate fruit peel could be exploited as a potential source of natural antimicrobial and antioxidant agents as well as tyrosinase inhibitors. PMID:23110485

Distribution of naphthenic acids in tissues of laboratory-exposed fish and in wild fishes from near the Athabasca oil sands in Alberta, Canada.

PubMed

Young, Rozlyn F; Michel, Lorelei Martínez; Fedorak, Phillip M

2011-05-01

Naphthenic acids, which have a variety of commercial applications, occur naturally in conventional crude oil and in highly biodegraded petroleum such as that found in the Athabasca oil sands in Alberta, Canada. Oil sands extraction is done using a caustic aqueous extraction process. The alkaline pH releases the naphthenic acids from the oil sands and dissolves them into water as their soluble naphthenate forms, which are anionic surfactants. These aqueous extracts contain concentrations of naphthenates that are acutely lethal to fishes and other aquatic organisms. Previous research has shown that naphthenic acids can be taken up by fish, but the distribution of these acids in various tissues of the fish has not been determined. In this study, rainbow trout (Oncorhynchus mykiss) were exposed to commercial (Merichem) naphthenic acids in the laboratory. After a 10-d exposure to approximately 3mg naphthenic acids/L, the fish were dissected and samples of gills, heart, liver, kidney, muscle, and eggs were extracted and analyzed for free (unconjugated) naphthenic acids by a gas chromatography-mass spectrometry method. Each of the tissues contained naphthenic acids and non-parametric statistical analyses showed that gills and livers contained higher concentrations than the muscles and that the livers had higher concentrations than the hearts. Four different species of fish (two fish of each species) were collected from the Athabasca River near two oil sands mining and extraction operations. No free naphthenic acids were detected in the muscle or liver of these fish. Copyright © 2010 Elsevier Inc. All rights reserved.

Method for extracting copper, silver and related metals

DOEpatents

Moyer, B.A.; McDowell, W.J.

1987-10-23

A process for selectively extracting precious metals such as silver and gold concurrent with copper extraction from aqueous solutions containing the same. The process utilizes tetrathiamacrocycles and high molecular weight organic acids that exhibit a synergistic relationship when complexing with certain metal ions thereby removing them from ore leach solutions.

Method for extracting copper, silver and related metals

DOEpatents

Moyer, Bruce A.; McDowell, W. J.

1990-01-01

A process for selectively extracting precious metals such as silver and gold concurrent with copper extraction from aqueous solutions containing the same. The process utilizes tetrathiamacrocycles and high molecular weight organic acids that exhibit a synergistic relationship when complexing with certain metal ions thereby removing them from ore leach solutions.

Wide-Scope Screening Method for Multiclass Veterinary Drug Residues in Fish, Shrimp, and Eel Using Liquid Chromatography-Quadrupole High-Resolution Mass Spectrometry.

PubMed

Turnipseed, Sherri B; Storey, Joseph M; Lohne, Jack J; Andersen, Wendy C; Burger, Robert; Johnson, Aaron S; Madson, Mark R

2017-08-30

A screening method for veterinary drug residues in fish, shrimp, and eel using LC with a high-resolution MS instrument has been developed and validated. The method was optimized for over 70 test compounds representing a variety of veterinary drug classes. Tissues were extracted by vortex mixing with acetonitrile acidified with 2% acetic acid and 0.2% p-toluenesulfonic acid. A centrifuged portion of the extract was passed through a novel solid phase extraction cartridge designed to remove interfering matrix components from tissue extracts. The eluent was then evaporated and reconstituted for analysis. Data were collected with a quadrupole-Orbitrap high-resolution mass spectrometer using both nontargeted and targeted acquisition methods. Residues were detected on the basis of the exact mass of the precursor and a product ion along with isotope pattern and retention time matching. Semiquantitative data analysis compared MS 1 signal to a one-point extracted matrix standard at a target testing level. The test compounds were detected and identified in salmon, tilapia, catfish, shrimp, and eel extracts fortified at the target testing levels. Fish dosed with selected analytes and aquaculture samples previously found to contain residues were also analyzed. The screening method can be expanded to monitor for an additional >260 veterinary drugs on the basis of exact mass measurements and retention times.

The Effect of Sericin from Various Extraction Methods on Cell Viability and Collagen Production

PubMed Central

Aramwit, Pornanong; Kanokpanont, Sorada; Nakpheng, Titpawan; Srichana, Teerapol

2010-01-01

Silk sericin (SS) can accelerate cell proliferation and attachment; however, SS can be extracted by various methods, which result in SS exhibiting different physical and biological properties. We found that SS produced from various extraction methods has different molecular weights, zeta potential, particle size and amino acid content. The MTT assay indicated that SS from all extraction methods had no toxicity to mouse fibroblast cells at concentrations up to 40 μg/mL after 24 h incubation, but SS obtained from some extraction methods can be toxic at higher concentrations. Heat-degraded SS was the least toxic to cells and activated the highest collagen production, while urea-extracted SS showed the lowest cell viability and collagen production. SS from urea extraction was severely harmful to cells at concentrations higher than 100 μg/mL. SS from all extraction methods could still promote collagen production in a concentration-dependent manner, even at high concentrations that are toxic to cells. PMID:20559510

Removal of toxic metals from vanadium-contaminated soils using a washing method: Reagent selection and parameter optimization.

PubMed

Jiang, Jianguo; Yang, Meng; Gao, Yuchen; Wang, Jiaming; Li, Dean; Li, Tianran

2017-08-01

Vanadium (V) contamination in soils is an increasing worldwide concern facing human health and environmental conservation. The fractionation of a metal influences its mobility and biological toxicity. We analyzed the fractionations of V and several other metals using the BCR three-step sequential extraction procedure. Among methods for removing metal contamination, soil washing is an effective permanent treatment. We conducted experiments to select the proper reagents and to optimize extraction conditions. Citric acid, tartaric acid, oxalic acid, and Na 2 EDTA all exhibited high removal rates of the extractable state of V. With a liquid-to-solid ratio of 10, washing with 0.4 mol/L citric acid, 0.4 mol/L tartaric acid, 0.4 mol/L oxalic acid, and 0.12 mol/L Na 2 EDTA led to removal rates of 91%, 88%, 88%, and 61%, respectively. The effect of multiple washing on removal rate was also explored. According to the changes observed in metal fractionations, differences in removal rates among reagents is likely associated with their pK a value, pH in solution, and chemical structure. We concluded that treating with appropriate washing reagents under optimal conditions can greatly enhance the remediation of vanadium-contaminated soils. Copyright © 2017 Elsevier Ltd. All rights reserved.

Amorphous titania modified with boric acid for selective capture of glycoproteins.

PubMed

Jin, Shanxia; Liu, Liping; Zhou, Ping

2018-05-22

Amorphous titania was modified with boric acid, and the resulting material was characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, X-ray powder diffraction and X-ray photoelectron spectrometry. The new material, in contrast to conventional boronate affinity materials containing boronic acid ligands, bears boric acid groups. It is shown to exhibit high specificity for glycoproteins, and this was applied to design a method for solid phase extraction of glycoproteins as shown for ribonuclease B, horse radish peroxidase and ovalbumin. Glycoproteins were captured under slightly alkaline environment and released in acidic solutions. The glycoproteins extracted were detected by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry. The binding capacities for ribonuclease B, horse radish peroxidase and ovalbumin typically are 9.3, 26.0 and 53.0 mg ∙ g -1 , respectively. The method was successfully applied to the selective enrichment of ovalbumin from egg white. Graphical abstract Schematic presentation of the capture of glycoproteins by amorphous titania modified with boric acid.

Chlorogenic acid stability in pressurized liquid extraction conditions.

PubMed

Wianowska, Dorota; Typek, Rafał; Dawidowicz, Andrzej L

2015-01-01

Chlorogenic acids (CQAs) are phenolic compounds naturally occurring in all higher plants. They are potentially useful in pharmaceuticals, foodstuffs, food additives, and cosmetics due to their recently suggested biomedical activity. Hence, research interest in CQA properties, their isomers, and natural occurrence has been growing. Pressurized liquid extraction (PLE) is regarded as an effective and quick sample preparation method in plant analysis. The short time of PLE decreases the risk of chemical degradation of extracted compounds, thus increasing the attractiveness of its application. However, PLE applied for plant sample preparation is not free from limitations. We found that trans-5-O-caffeoylquinic acid (trans-5-CQA), the main CQA isomer, isomerizes to 3- and 4-O-caffeoylquinic acids and undergoes transesterification, hydrolysis, and reaction with water even in rapid PLE. Moreover, the number and concentration of trans-5-CQA derivatives formed in PLE strongly depends on extractant composition, its pH, and extraction time and temperature. It was not possible to find the PLE conditions in which the transformation process of trans-5-CQA would be eliminated.

Extraction of High Quality DNA from Seized Moroccan Cannabis Resin (Hashish)

PubMed Central

El Alaoui, Moulay Abdelaziz; Melloul, Marouane; Alaoui Amine, Sanaâ; Stambouli, Hamid; El Bouri, Aziz; Soulaymani, Abdelmajid; El Fahime, Elmostafa

2013-01-01

The extraction and purification of nucleic acids is the first step in most molecular biology analysis techniques. The objective of this work is to obtain highly purified nucleic acids derived from Cannabis sativa resin seizure in order to conduct a DNA typing method for the individualization of cannabis resin samples. To obtain highly purified nucleic acids from cannabis resin (Hashish) free from contaminants that cause inhibition of PCR reaction, we have tested two protocols: the CTAB protocol of Wagner and a CTAB protocol described by Somma (2004) adapted for difficult matrix. We obtained high quality genomic DNA from 8 cannabis resin seizures using the adapted protocol. DNA extracted by the Wagner CTAB protocol failed to give polymerase chain reaction (PCR) amplification of tetrahydrocannabinolic acid (THCA) synthase coding gene. However, the extracted DNA by the second protocol permits amplification of THCA synthase coding gene using different sets of primers as assessed by PCR. We describe here for the first time the possibility of DNA extraction from (Hashish) resin derived from Cannabis sativa. This allows the use of DNA molecular tests under special forensic circumstances. PMID:24124454

Magnetic covalent triazine-based frameworks as magnetic solid-phase extraction adsorbents for sensitive determination of perfluorinated compounds in environmental water samples.

PubMed

Ren, Ji-Yun; Wang, Xiao-Li; Li, Xiao-Li; Wang, Ming-Lin; Zhao, Ru-Song; Lin, Jin-Ming

2018-02-01

Covalent organic frameworks (COFs), which are a new type of carbonaceous polymeric material, have attracted great interest because of their large surface area and high chemical and thermal stability. However, to the best of our knowledge, no work has reported the use of magnetic COFs as adsorbents for magnetic solid-phase extraction (MSPE) to enrich and determine environmental pollutants. This work aims to investigate the feasibility of using covalent triazine-based framework (CTF)/Fe 2 O 3 composites as MSPE adsorbents to enrich and analyze perfluorinated compounds (PFCs) at trace levels in water samples. Under the optimal conditions, the method developed exhibited low limits of detection (0.62-1.39 ng·L -1 ), a wide linear range (5-4000 ng L -1 ), good repeatability (1.12-9.71%), and good reproducibility (2.45-7.74%). The new method was successfully used to determine PFCs in actual environmental water samples. MSPE based on CTF/Fe 2 O 3 composites exhibits potential for analysis of PFCs at trace levels in environmental water samples. Graphical abstract Magnetic covalent triazine-based frameworks (CTFs) were used as magnetic solid-phase extraction adsorbents for the sensitive determination of perfluorinated compounds in environmental water samples. PFBA perfluorobutyric acid, PFBS perfluorobutane sulfonate, PFDA perfluorodecanoic acid, PFDoA perfluorododecanoic acid, PFHpA perfluoroheptanoic acid, PFHxA perfluorohexanoic acid, PFHxS perfluorohexane sulfonate, PFNA perfluorononanoic acid, PFOA perfluorooctanoic acid, PFPeA perfluoropentanoic acid, PFUdA Perfluoroundecanoic acid.

The high-performance liquid chromatography/multistage electrospray mass spectrometric investigation and extraction optimization of beech (Fagus sylvatica L.) bark polyphenols.

PubMed

Hofmann, Tamás; Nebehaj, Esztella; Albert, Levente

2015-05-08

The aim of the present work was the high-performance liquid chromatographic separation and multistage mass spectrometric characterization of the polyphenolic compounds of beech bark, as well as the extraction optimization of the identified compounds. Beech is a common and widely used material in the wood industry, yet its bark is regarded as a by-product. Using appropriate extraction methods these compounds could be extracted and utilized in the future. Different extraction methods (stirring, sonication, microwave assisted extraction) using different solvents (water, methanol:water 80:20 v/v, ethanol:water 80:20 v/v) and time/temperature schedules have been compared basing on total phenol contents (Folin-Ciocâlteu) and MRM peak areas of the identified compounds to investigate optimum extraction efficiency. Altogether 37 compounds, including (+)-catechin, (-)-epicatechin, quercetin-O-hexoside, taxifolin-O-hexosides (3), taxifolin-O-pentosides (4), B-type (6) and C-type (6) procyanidins, syringic acid- and coumaric acid-di-O-glycosides, coniferyl alcohol- and sinapyl alcohol-glycosides, as well as other unknown compounds with defined [M-H](-) m/z values and MS/MS spectra have been tentatively identified. The choice of the method, solvent system and time/temperature parameters favors the extraction of different types of compounds. Pure water can extract compounds as efficiently as mixtures containing organic solvents under high-pressure and high temperature conditions. This supports the implementation of green extraction methods in the future. Extraction times that are too long and high temperatures can result in the decrease of the concentrations. Future investigations will focus on the evaluation of the antioxidant capacity and utilization possibilities of the prepared extracts. Copyright © 2015 Elsevier B.V. All rights reserved.

Green extraction of grape skin phenolics by using deep eutectic solvents.

PubMed

Cvjetko Bubalo, Marina; Ćurko, Natka; Tomašević, Marina; Kovačević Ganić, Karin; Radojčić Redovniković, Ivana

2016-06-01

Conventional extraction techniques for plant phenolics are usually associated with high organic solvent consumption and long extraction times. In order to establish an environmentally friendly extraction method for grape skin phenolics, deep eutectic solvents (DES) as a green alternative to conventional solvents coupled with highly efficient microwave-assisted and ultrasound-assisted extraction methods (MAE and UAE, respectively) have been considered. Initially, screening of five different DES for proposed extraction was performed and choline chloride-based DES containing oxalic acid as a hydrogen bond donor with 25% of water was selected as the most promising one, resulting in more effective extraction of grape skin phenolic compounds compared to conventional solvents. Additionally, in our study, UAE proved to be the best extraction method with extraction efficiency superior to both MAE and conventional extraction method. The knowledge acquired in this study will contribute to further DES implementation in extraction of biologically active compounds from various plant sources. Copyright © 2016 Elsevier Ltd. All rights reserved.

Development and validation of two methods based on high-performance liquid chromatography-tandem mass spectrometry for determining 1,2-benzopyrone, dihydrocoumarin, o-coumaric acid, syringaldehyde and kaurenoic acid in guaco extracts and pharmaceutical preparations.

PubMed

Gasparetto, João C; de Francisco, Thais M Guimarães; Campos, Francinete R; Pontarolo, Roberto

2011-04-01

In this study, two HPLC-ESI-MS/MS methods were developed and validated for the determination of 1,2-benzopyrone (COU), o-coumaric acid (OCA), kaurenoic acid (KAU), syringaldehyde (SYR), and dihydrocoumarin (DIH) in guaco extracts and pharmaceutical preparations (syrup and oral solution). The chromatographic separation was achieved using a C18 XBridge 150×2.1-mm (5-μm particle size) column maintained at 25°C. The mobile phases consisted of a gradient of water and acetonitrile containing 0.05% formic acid or 5  mM ammonium formate for the positive and negative ion modes, respectively. All of the calibration curves showed excellent coefficients of correlation (r≥0.9970) over the ranges of 1.25-400  ng/mL for coumarin, 10-600  ng/mL for dihydrocoumarin, 5-250  ng/mL for KAU, and 25-500  ng/mL for o-coumaric acid and syringaldehyde. The range of recovery was 96.3-103% with an RSD% of <4.85% for intraday and interday precision. The results indicate that the developed methods are fast, efficient, and sensitive for the quantification of the guaco metabolites in extracts and pharmaceutical forms while avoiding purification and derivatization steps. Copyright © 2011 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Determination of phthalates released from paper packaging materials by solid-phase extraction-high-performance liquid chromatography.

PubMed

Gao, Xin; Yang, Bofeng; Tang, Zhixu; Luo, Xin; Wang, Fengmei; Xu, Hui; Cai, Xue

2014-01-01

A solid phase extraction (SPE) high-performance liquid chromatography (HPLC) method was developed for the simultaneous determination of 10 phthalic acid esters (dimethyl phthalate, diethyl phthalate, dipropyl phthalate, benzylbutyl phthalate, diisobutyl phthalate, dicyclohexyl phthalate, diamyl phthalate, di-n-hexyl phthalate, di-n-octyl phthalate and di-2-ethylhexyl phthalate) released from food paper packaging materials. The use of distilled water, 3% acetic acid (w/v), 10% ethanol (v/v) and 95% ethanol (v/v) instead of the different types of food simulated the migration of 10 phthalic acid esters from food paper packaging materials; the phthalic acid esters in four food simulants were enriched and purified by a C18 SPE column and nitrogen blowing, and quantified by HPLC with a diode array detector. The chromatographic conditions and extraction conditions were optimized and all 10 of the phthalate acid esters had a maximum absorbance at 224 nm. The method showed limitations of detection in the range of 6.0-23.8 ng/mL the correlation coefficients were greater than 0.9999 in all cases, recovery values ranged between 71.27 and 106.97% at spiking levels of 30, 60 and 90 ng/mL and relative standard deviation values ranged from 0.86 to 8.00%. The method was considered to be simple, fast and reliable for a study on the migration of these 10 phthalic acid esters from food paper packaging materials into food.

Rapid and sensitive detection of the phenoxy acid herbicides in environmental water samples by magnetic solid-phase extraction combined with liquid chromatography-tandem mass spectrometry.

PubMed

Peng, Mao-Min; Han, Ya-Quan; Xia, Hong; Hu, Xi-Zhou; Zhou, You-Xiang; Peng, Li-Jun; Peng, Xi-Tian

2018-05-01

Phenoxy acid herbicides are widely used herbicides that play an important role in improving the yield and quality of crops. However, some research has shown that this kind of herbicide is poisonous to human and animals. In this study, a rapid and sensitive method was developed for the detection of seven phenoxy acid herbicides in water samples based on magnetic solid-phase extraction followed by liquid chromatography and tandem mass spectrometry. Magnetic amino-functionalized multiwalled carbon nanotubes were prepared by mixing bare magnetic Fe 3 O 4 nanoparticles with commercial amino-functionalized multiwalled carbon nanotubes in water. Then the amino-functionalized multiwalled carbon nanotubes were used to enrich phenoxy acid herbicides from water samples based on hydrophobic and ionic interactions. The effects of experimental variables on the extraction efficiency have been studied in detail. Under the optimized conditions, the method validation was performed. Good linearities for seven phenoxy acid herbicides were obtained with squared regression coefficients ranging from 0.9971 to 0.9989. The limits of detection ranged from 0.01 to 0.02 μg/L. The method recoveries of seven phenoxy acid herbicides spiked at three concentration levels in a blank sample were from 92.3 to 103.2%, with inter- and intraday relative standard deviations less than 12.6%. © 2018 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Extraction and Determination of Trace Amounts of p-Coumaric Acid in Vinegar, Carrot Juice, and Seed Extract from Silybum marianum (L.) Gaertn.

PubMed

Khani, Rouhollah; Rostami, Zeinab; Bagherzade, Ghodsieh; Khojeh, Vahid

2018-03-01

In this study, for the monitoring and quantification of p-coumaric acid (p-CA) in vinegar, carrot juice, and seed extract from the plant species Silybum marianum (L.) Gaertn, an efficient and low-cost analytical method has been applied. For this purpose, a dispersive liquid-liquid microextraction (DLLME) method, followed by UV-Vis spectrophotometric detection, was used. To form a cloudy solution, a binary mixture containing ethanol as a disperser solvent and chloroform as an extraction solvent was rapidly injected by syringe into a sample solution containing p-CA. After centrifugation, dilution of the obtained organic phase was done with the proper amount of ethanol, and the phase was transferred into a micro cell for subsequent measurement. Some effective parameters for the DLLME method, such as the volume of disperser solvent and extraction solvent, pH, and salt concentration were inspected by a 24 full factorial central composite design using design Export Software. Under the optimized conditions, linearity was between 10 and 150 ng/mL, and the LOD was 2.3 ng/mL. The results of the proposed method were similar to the obtained results using a GC with flame-ionization detection method.

Simultaneous Determination of Perfluorinated Compounds in Edible Oil by Gel-Permeation Chromatography Combined with Dispersive Solid-Phase Extraction and Liquid Chromatography-Tandem Mass Spectrometry.

PubMed

Yang, Lili; Jin, Fen; Zhang, Peng; Zhang, Yanxin; Wang, Jian; Shao, Hua; Jin, Maojun; Wang, Shanshan; Zheng, Lufei; Wang, Jing

2015-09-30

A simple analytical method was developed for the simultaneous analysis of 18 perfluorinated compounds (PFCs) in edible oil. The target compounds were extracted by acetonitrile, purified by gel permeation chromatography (GPC) and dispersive solid-phase extraction (DSPE) using graphitized carbon black (GCB) and octadecyl (C18), and analyzed by liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ES-MS/MS) in negative ion mode. Recovery studies were performed at three fortification levels. The average recoveries of all target PFCs ranged from 60 to 129%, with an acceptable relative standard deviation (RSD) (1-20%, n = 3). The method detection limits (MDLs) ranged from 0.004 to 0.4 μg/kg, which was significantly improved compared with the existing liquid-liquid extraction and cleanup method. The method was successfully applied for the analysis of all target PFCs in edible oil samples collected from markets in Beijing, China, and the results revealed that C6-C10 perfluorocarboxylic acid (PFCAs) and C7 perfluorosulfonic acid PFSAs were the major PFCs detected in oil samples.

A new multiplex method for the diagnosis of peroxisomal disorders allowing simultaneous determination of plasma very-long-chain fatty acids, phytanic, pristanic, docosahexaenoic and bile acids by high-performance liquid chromatography-atmospheric pressure chemical ionization-tandem mass spectrometry.

PubMed

Semeraro, Michela; Rizzo, Cristiano; Boenzi, Sara; Cappa, Marco; Bertini, Enrico; Antonetti, Giacomo; Dionisi-Vici, Carlo

2016-07-01

Peroxisomal disorders (PDs) present with wide phenotypic variability. An appropriate diagnosis requires a complete analysis of peroxisomal metabolites. We developed a multiplex LC-MS/MS method, using atmospheric pressure chemical ionization allowing the simultaneous determination in plasma of very-long-chain fatty acids, phytanic, pristanic, docosahexaenoic acids and di- and tri-hydroxycolestanoic bile acids. Two hundred microliters of plasma extracted with acetonitrile and 200μl extracted with hexane after an acid hydrolysis were combined, evaporated, dissolved in 10μl of methanol and analyzed. The acquisition was in negative-ion mode using multiple reaction monitoring. The method was validated analytically and clinically. Linearity was 0.1-200μmol/l for docosanoic, cis-13-docosenoic, tetracosanoic, cis-15-tetracosenoic and phytanic acids; 0.01-10μmol/l for hexacosanoic acid; 0.02-20μmol/l for di-hydroxycolestanoic, tri-hydroxycolestanoic and pristanic acids; 0.3-300μmol/l for docosahexaenoic acid. Intra-day and inter-day CVs were below 3.88 and 3.98 respectively for all compounds. Samples from patients with known peroxisomal disorders were compared with controls and the method allowed to confirm the diagnosis in all subjects with a 100% sensitivity. The advantage of this multiplex method is to allow in a single chromatographic run the simultaneous determination of a large number of peroxisome biomarkers with a simple preparative phase without derivatization. Copyright © 2016 Elsevier B.V. All rights reserved.

Comparative Evaluation of Three Homogenization Methods for Isolating Middle East Respiratory Syndrome Coronavirus Nucleic Acids From Sputum Samples for Real-Time Reverse Transcription PCR

PubMed Central

Yong, Dongeun; Ki, Chang-Seok; Kim, Jae-Seok; Seong, Moon-Woo; Lee, Hyukmin

2016-01-01

Background Real-time reverse transcription PCR (rRT-PCR) of sputum samples is commonly used to diagnose Middle East respiratory syndrome coronavirus (MERS-CoV) infection. Owing to the difficulty of extracting RNA from sputum containing mucus, sputum homogenization is desirable prior to nucleic acid isolation. We determined optimal homogenization methods for isolating viral nucleic acids from sputum. Methods We evaluated the following three sputum-homogenization methods: proteinase K and DNase I (PK-DNase) treatment, phosphate-buffered saline (PBS) treatment, and N-acetyl-L-cysteine and sodium citrate (NALC) treatment. Sputum samples were spiked with inactivated MERS-CoV culture isolates. RNA was extracted from pretreated, spiked samples using the easyMAG system (bioMérieux, France). Extracted RNAs were then subjected to rRT-PCR for MERS-CoV diagnosis (DiaPlex Q MERS-coronavirus, SolGent, Korea). Results While analyzing 15 spiked sputum samples prepared in technical duplicate, false-negative results were obtained with five (16.7%) and four samples (13.3%), respectively, by using the PBS and NALC methods. The range of threshold cycle (Ct) values observed when detecting upE in sputum samples was 31.1–35.4 with the PK-DNase method, 34.7–39.0 with the PBS method, and 33.9–38.6 with the NALC method. Compared with the control, which were prepared by adding a one-tenth volume of 1:1,000 diluted viral culture to PBS solution, the ranges of Ct values obtained by the PBS and NALC methods differed significantly from the mean control Ct of 33.2 (both P<0.0001). Conclusions The PK-DNase method is suitable for homogenizing sputum samples prior to RNA extraction. PMID:27374711

Antimicrobial activity of hop extracts against foodborne pathogens for meat applications.

PubMed

Kramer, B; Thielmann, J; Hickisch, A; Muranyi, P; Wunderlich, J; Hauser, C

2015-03-01

The objective of this study was the fundamental investigation of the antimicrobial efficiency of various hop extracts against selected foodborne pathogens in vitro, as well as their activity against Listeria monocytogenes in a model meat marinade and on marinated pork tenderloins. In a first step, the minimum inhibitory concentrations (MIC) of three hop extracts containing either α- or β-acids or xanthohumol were determined against test bacteria including L. monocytogenes, Staphylococcus aureus, Salmonella enterica and Escherichia coli by a colorimetric method based on the measurement of bacterial metabolic activity. Moreover, the influence of either lactic or citric acid on the antimicrobial activity of the hop extracts was evaluated. The efficiency of hop extracts as a natural food preservative was then tested in a model meat marinade at 2 and 8°C, respectively, and finally on marinated pork. The experiments showed that Gram-positive bacteria were strongly inhibited by hop extracts containing β-acids and xanthohumol (MIC values of 6.3 and 12.5 ppm, respectively), whereas the antimicrobial activity of the investigated α-acid extract was significantly lower (MIC values of 200 ppm). Gram-negative bacteria were highly resistant against all tested hop extracts. Acidification of the test media led to a decrease of the MIC values. The inhibitory activity of the hop extracts against L. monocytogenes was strongly reduced in a fat-containing model meat marinade, but the efficiency of β-acids in this matrix could be increased by lowering pH and storage temperatures. By applying 0.5 % β-acids at pH = 5 in a model marinade, the total aerobic count of pork tenderloins was reduced up to 0.9 log10 compared with marinated pork without hop extract after 2 weeks of storage at 5°C. β-acid containing hop extracts have proven to possess a high antimicrobial activity against Gram-positive bacteria in vitro and in a practice-related application for food preservation. Antimicrobial hop extracts could be used as natural preservatives in food applications to extend the shelf life and to increase the safety of fresh products. © 2014 The Society for Applied Microbiology.

Dispersive liquid-liquid microextraction combined with microwave-assisted derivatization for determining lipoic acid and its metabolites in human urine.

PubMed

Tsai, Chia-Ju; Chen, Yen-Ling; Feng, Chia-Hsien

2013-10-04

This study explored dispersive liquid-liquid microextraction for extraction and concentration of lipoic acid in human urine. To improve the detection of lipoic acid by both capillary liquid chromatography (CapLC) with UV detection and matrix-assisted laser desorption ionization time-of-flight mass spectrometry (MALDI-TOF MS), microwave-assisted derivatization with 4-bromomethyl-6,7-dimethoxycoumarin was performed to render lipoic acid chromophores for UV detection and also high ionization efficiency in MALDI. All parameters that affected lipoic acid extraction and derivatization from urine were investigated and optimized. In the analyses of human urine samples, the two methods had a linear range of 0.1-20 μM with a correlation coefficient of 0.999. The detection limits of CapLC-UV and MALDI-TOF MS were 0.03 and 0.02 μM (S/N ≧ 3), respectively. The major metabolites of lipoic acid, including 6,8-bismethylthio-octanoic acid, 4,6-bismethylthio-hexanoic acid, and 2,4-bismethylthio-butanoic acid were also extracted by dispersive liquid-liquid microextraction and detected by MALDI-TOF MS. The minor metabolites (undetectable by MALDI-TOF MS), bisnorlipoic acid and tetranorlipoic acid were also extracted by dispersive liquid-liquid microextraction and identified with an LTQ Orbitrap mass spectrometer. After dispersive liquid-liquid microextraction and microwave-assisted derivatization, all lipoic acid derivatizations and metabolites were structurally confirmed by LTQ Orbitrap. Copyright © 2013 Elsevier B.V. All rights reserved.

High-pressure liquid chromatographic analysis of pramoxine hydrochloride in high lipoid aerosol foam dosage form.

PubMed

Weinberger, R; Mann, B; Posluszny, J

1980-04-01

A rapid and quantitative method for the determination of pramoxine hydrochloride by high-pressure liquid chromatography is presented. The drug is extracted as the salt from a preparation with a high lipoid composition by partitioning it to the aqueous phase of an ether-methanol-water-acetic acid system. The extract is chromatographed on an octadecylsilane bonded packing with a methanol-water-acetic acid-methanesulfonic acid mobile phase. The time required for each separation is approximately 6 min. Analytical recoveries of 100.4 +/- 1.5% were obtained.

Gas chromatographic-mass spectrometric determination of alkylphosphonic acids from aqueous samples by ion-pair solid-phase extraction on activated charcoal and methylation.

PubMed

Vijaya Saradhi, U V R; Prabhakar, S; Jagadeshwar Reddy, T; Murty, M R V S

2007-07-20

In the present paper, we report an improved ion-pair solid-phase extraction (IP-SPE) method for the analysis of alkylphosphonic acids, namely, methyl, ethyl and propylphosphonic acids, present in the aqueous sample. The aqueous sample was mixed with an ion-pair reagent, phenyltrimethylammonium hydroxide (PTMAH) and passed through activated charcoal SPE cartridge. The retained chemicals in the cartridge were extracted with methanol and analysed by gas chromatography-mass spectrometry (GC-MS) under the electron impact ionization (EI) mode. The analytes were converted to their methyl esters by pyrolytic methylation in the hot GC injection port. The recoveries of alkylphosphonic acids were above 95% and the minimum detection limits were as low as 10 ng/mL. The recovery of the test chemicals was tested with solvents, dichloromethane, n-hexane, ethyl acetate, acetone, acetonitrile and methanol. The chemicals could be efficiently extracted by the hydrophilic solvents. The method did not work at the highly acidic pH (when acidified with dilute HCl) but worked well from pH 4.0 to 14.0. The present method was also tested with other tetra-(methyl, ethyl, propyl and n-butyl)ammonium hydroxides. The test chemicals were not converted to their methyl and ethyl esters with tetramethyl and tetraethylammonium hydroxides, whereas they were converted to their corresponding propyl and n-butyl esters with tetrapropyl and tetra(n-butyl)ammonium hydroxides. The method was also applied to two highly cross-linked polymeric sorbents DSC-6S and Oasis HLB. The recovery of the chemicals on these sorbents was observed to be poor. Methylation using phenyltrimethylammonium hydroxide is non-hazardous and advantageous over methylation using diazomethane. The method was applied to the analysis of aqueous samples given in one of the official proficiency tests conducted by the Organization for the Prohibition of Chemical Weapons and all the spiked chemicals were identified as methyl esters.

Effect of various domestic processing and cooking methods on phytic acid and HCl-extractability of calcium, phosphorus and iron of pigeon pea.

PubMed

Duhan, A; Khetarpaul, N; Bishnoi, S

1999-01-01

Manak, the high yielding cultivator of pigeon pea (Cajanus cajan) released by (International Crop Research Institute for Semi-Arid Tropics) ICRISAT, India was subjected to various domestic processing and cooking methods viz., soaking (6, 12 and 18 h, 30 degrees C), soaking and dehulling, ordinary cooking, pressure cooking and germination (24, 36 and 48 h, 30 degrees C). The unprocessed seeds of this variety contained considerable amounts of phytic acid i.e. 917 mg per 100 g. This antinutrient was reduced significantly (P < 0.05) to varying extents (4-37%) in the processed samples. Except soaking and dehulling, the remaining processing and cooking methods did not lower the contents of total calcium, phosphorus and iron. That HCl-extractability of these dietary essential minerals, an index of their bioavailability, enhanced significantly when the pigeon pea seeds were processed and cooked, may be due to reduction in phytate content, which is known to chelate the minerals. A significant and negative correlation between the phytic acid and HCl-extractability of minerals further strengthens our findings.

One-Step Extraction and Hydrolysis of Flavonoid Glycosides in Rape Bee Pollen Based on Soxhlet-Assisted Matrix Solid Phase Dispersion.

PubMed

Tu, Xijuan; Ma, Shuangqin; Gao, Zhaosheng; Wang, Jing; Huang, Shaokang; Chen, Wenbin

2017-11-01

Flavonoids are frequently found as glycosylated derivatives in plant materials. To determine contents of flavonoid aglycones in these matrices, procedures for the extraction and hydrolysis of flavonoid glycosides are required. The current sample preparation method is both labour and time consuming. Develop a modified matrix solid phase dispersion (MSPD) procedure as an alternative methodology for the one-step extraction and hydrolysis of flavonoid glycosides. HPLC-DAD was applied for demonstrating the one-step extraction and hydrolysis of flavonoids in rape bee pollen. The obtained contents of flavonoid aglycones (quercetin, kaempferol, isorhamnetin) were used for the optimisation and validation of the method. The extraction and hydrolysis were accomplished in one step. The procedure completes in 2 h with silica gel as dispersant, a 1:2 ratio of sample to dispersant, and 60% aqueous ethanol with 0.3 M hydrochloric acid as the extraction solution. The relative standard deviations (RSDs) of repeatability were less than 5%, and the recoveries at two fortified levels were between 88.3 and 104.8%. The proposed methodology is simple and highly efficient, with good repeatability and recovery. Compared with currently available methods, the present work has advantages of using less time and labour, higher extraction efficiency, and less consumption of the acid catalyst. This method may have applications for the one-step extraction and hydrolysis of bioactive compounds from plant materials. Copyright © 2017 John Wiley & Sons, Ltd. Copyright © 2017 John Wiley & Sons, Ltd.

Combined quantification of faecal sterols, stanols, stanones and bile acids in soils and terrestrial sediments by gas chromatography-mass spectrometry.

PubMed

Birk, Jago Jonathan; Dippold, Michaela; Wiesenberg, Guido L B; Glaser, Bruno

2012-06-15

Faeces incorporation can alter the concentration patterns of stanols, stanones, Δ(5)-sterols and bile acids in soils and terrestrial sediments. A joint quantification of these substances would give robust and specific information about the faecal input. Therefore, a method was developed for their purification and determination via gas chromatography-mass spectrometry (GC-MS) based on a total lipid extract (TLE) of soils and terrestrial sediments. Stanols, stanones, Δ(5)-steroles and bile acids were extracted by a single Soxhlet extraction yielding a TLE. The TLE was saponified with KOH in methanol. Sequential liquid-liquid extraction was applied to recover the biomarkers from the saponified extract and to separate the bile acids from the neutral stanoles, stanones and Δ(5)-steroles. The neutral fraction was directly purified using solid phase extraction (SPE) columns packed with 5% deactivated silica gel. The bile acids were methylated in dry HCl in methanol and purified on SPE columns packed with activated silica gel. A mixture of hexamethyldisilazane (HMDS), trimethylchlorosilane (TMCS) and pyridine was used to silylate the hydroxyl groups of the stanols and Δ(5)-sterols avoiding a silylation of the keto groups of the stanones in their enol-form. Silylation of the bile acids was carried out with N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA) containing N-trimethylsilylimidazole (TSIM). TLEs from a set of soils with different physico-chemical properties were used for method evaluation and for comparison of amounts of faecal biomarkers analysed with saponification and without saponification of the TLE. Therefore, a Regosol, a Podzol and a Ferralsol were sampled. To proof the applicability of the method for faecal biomarker analyses in archaeological soils and sediments, additional samples were taken from pre-Columbian Anthrosols in Amazonia and an Anthrosol from a site in central Europe settled since the Neolithic. The comparison of the amounts of steroids in combination with and without saponification of the TLE showed that high amounts of faecal biomarkers occur bound to other lipids and were liberated by saponification. The method was evaluated by standard addition. The standard contained 5β-stanols, 5β-stanones and their 5α-isomers together with Δ(5)-sterols and bile acids (19 substances). The standard addition revealed mean recoveries of individual substances ≥85%. The recoveries of biomarkers within each biomarker group did not differ significantly. Precisions were ≤0.22 (RSD) and quantification limits were between 1.3 and 10 ng g(-1) soil. These data showed that the method can be applied for quantification of trace amounts of faecal steroids and for the analyses of steroid patterns to detect enhanced faeces deposition in soils and sediments. Copyright © 2012 Elsevier B.V. All rights reserved.

Quantitation of zoledronic acid in murine bone by liquid chromatography coupled with tandem mass spectrometry.

PubMed

Raccor, Brianne S; Sun, Jianxun; Lawrence, Ross F; Li, Lei; Zhang, Hai; Somerman, Martha J; Totah, Rheem A

2013-09-15

An in vitro method for extraction and quantification of zoledronic acid (ZA) from murine bone was developed. Whole mouse bones were incubated in ZA solutions with predetermined concentrations and bound ZA was subsequently extracted from bone with phosphoric acid and derivatized using trimethylsilyl diazomethane (TMS-DAM). ZA tetra-methyl phosphonate was quantified by liquid chromatography coupled with tandem mass spectrometry (LC/MS/MS). This resulted in a sensitive, accurate, and precise method that was linear over three orders of magnitude (0.0250-50.0μg/mL ZA). For quality control (QC) samples, intra-and inter-day coefficients of variance were calculated and were less than 10%. This method was then applied to an in vivo model to quantitate ZA from the femur and mandible of three mice treated with ZA for two weeks. The mean ZA extracted from the mandible was four fold higher than that extracted from the femur (3.06±0.52 vs. 0.76±0.09ng/mg, respectively) indicating that ZA did not distribute equally in the skeleton and had a preference to the mandible. In conclusion, a highly sensitive method to measure ZA from mouse skeleton was developed, which can be easily adapted to multiple mammalian models including humans receiving ZA treatment. Copyright © 2013 Elsevier B.V. All rights reserved.

Screening Natural Content of Water-Soluble B Vitamins in Fish: Enzymatic Extraction, HILIC Separation, and Tandem Mass Spectrometric Determination.

PubMed

Chatterjee, Niladri Sekhar; Kumar, K Ashok; Ajeeshkumar, K K; Kumari, K R Remya; Vishnu, K V; Anandan, Rangasamy; Mathew, Suseela; Ravishankar, C N

2017-05-01

Despite the potential of LC with tandem MS (MS/MS) in improving sensitivity and selectivity, analytical methods are scarce for the determination of protein-bound and phosphorylated forms of B vitamins in food. This prompted us to develop a method for LC-MS/MS determination of naturally occurring nicotinamide, nicotinic acid, thiamine, pyridoxine, riboflavin, pantothenic acid, biotin, folic acid, and cyanocobalamin in fish. Baseline separation of the vitamins was achieved in a hydrophilic interaction LC condition. An ultrasonication-assisted enzymatic extraction protocol for sample preparation was optimized and validated. The time required for extraction was significantly reduced (to 4 h), while maintaining good extraction efficiency. Acetonitrile content (80%, v/v) in the prepared sample was found to be optimum for excellent peak shape and sensitivity. The dynamic linear range of the vitamins ranged from 2.5 to 500 ng/g, and the regression coefficient values were greater than 0.99. LOQ values ranged from 0.4 to 50 ng/g for the different vitamins. The spike recovery values at 50 and 100 ng/g ranged from 87.5 to 97.5%. The intra- and interday precision values were satisfactory. Accuracy of the developed method was determined by analysis of a Certified Reference Material. The method could also be used for unambiguous determination of the natural content of the target vitamins in fish.

Liquid chromatograpic-mass spectrometric analysis of phenolics and free radical scavenging activity of rosemary extract from different raw material.

PubMed

Almela, Luis; Sánchez-Muñoz, Blas; Fernández-López, José A; Roca, María J; Rabe, Virginia

2006-07-07

The antioxidant activity of rosemary (Rosmarinus officinalis) extract from different raw materials has been studied. Extracts were prepared from wild or drip-irrigated plants, as well as from the by-product resulting from the distillation of the aromatic essential oil. The radical scavenging activity of rosemary extracts was compared with that of antioxidants widely used in food, such as BHT and delta-tocopherol, using an optimization of the method based on the reduction of the radical 2,2-diphenyl-1-picrylhydrazyl (DPPH). The results pointed the excellent antioxidant activity of the crude fresh rosemary extracts, which was almost identical to that of pure delta-tocopherol, and higher than that of BHT; extracts prepared from distilled rosemary showed the lowest activity, although they are also of interest due to the low cost of the raw material. High performance liquid chromatography (HPLC) combined with diode array (DAD) and electrospray (ESI)-ion trap-MS detection was used to separate and identify the compounds present in the rosemary extracts. Rosmarinic acid, carnosic acid and seven of their terpene-type metabolites, and seven flavones were identified. The drying and/or distillation treatments used with the plant material strongly affected the content of the two compounds of higher antioxidant activity: rosmarinic acid and carnosic acid.

Anti-inflammatory activity of extract and fractions from Nepeta sibthorpii Bentham.

PubMed

Miceli, N; Taviano, M F; Giuffrida, D; Trovato, A; Tzakou, O; Galati, E M

2005-02-28

Several species of Nepeta genus are utilized in folk medicine for treatment of contusions, rheumatic pains, fever, cutaneous eruptions. Some species are employed for their anti-inflammatory properties. In this paper, we report the results of phytochemical studies on aerial parts of Nepeta sibthorpii Bentham (Lamiaceae), an endemic plant of Greece. The bioassay-guided fractionation of methanol extract led to the isolation of ursolic acid and polyphenol fraction. By HPLC, we determined some phenolics: chlorogenic acid (0.315 mg/g) and the flavonoids rutin (0.091 mg/g), luteolin-7-O-glucoside (0.387 mg/g) and a luteolin derivative. We assayed the radical scavenging activity of Nepeta sibthorpii methanol extract by the 1,1-diphenyl-2-picrylhydrazyl (DPPH) method. Moreover, we studied the anti-inflammatory activity of Nepeta sibthorpii methanol extract (50 mg/kg, os), ursolic acid and polyphenol fraction (dose corresponding to 50 mg/kg of methanol extract, os) in the carrageenan-induced paw oedema in rat. In this experimental model, we observed a significant inhibition of paw oedema. We suppose that the anti-inflammatory effect of methanol extract could be related to the free radical scavenging activity and that it depends on a synergic action of all the components of the methanol extract, even if ursolic acid can be considered the main responsible for this activity.