scholarly journals Analytical Technique Optimization on the Detection of β-cyclocitral in Microcystis Species

Molecules ◽  
2020 ◽  
Vol 25 (4) ◽  
pp. 832
Author(s):  
Ryuji Yamashita ◽  
Beata Bober ◽  
Keisuke Kanei ◽  
Suzue Arii ◽  
Kiyomi Tsuji ◽  
...  

β-Cyclocitral, specifically produced by Microcystis, is one of the volatile organic compounds (VOCs) derived from cyanobacteria and has a lytic activity. It is postulated that β-cyclocitral is a key compound for regulating the occurrence of cyanobacteria and related microorganisms in an aquatic environment. β-Cyclocitral is sensitively detected when a high density of the cells is achieved from late summer to autumn. Moreover, it is expected to be involved in changes in the species composition of cyanobacteria in a lake. Although several analysis methods for β-cyclocitral have already been reported, β-cyclocitral could be detected using only solid phase micro-extraction (SPME), whereas it could not be found at all using the solvent extraction method in a previous study. In this study, we investigated why β-cyclocitral was detected using only SPME GC/MS. Particularly, three operations in SPME, i.e., extraction temperature, sample stirring rate, and the effect of salt, were examined for the production of β-cyclocitral. Among these, heating (60 °C) was critical for the β-cyclocitral formation. Furthermore, acidification with a 1-h storage was more effective than heating when comparing the obtained amounts. The present results indicated that β-cyclocitral did not exist as the intact form in cells, because it was formed by heating or acidification of the resulting intermediates during the analysis by SPME. The obtained results would be helpful to understand the formation and role of β-cyclocitral in an aquatic environment.

Author(s):  
Antonia Flores ◽  
Silvia Sorolla ◽  
Concepció Casas ◽  
Rosa Cuadros ◽  
Anna Bacardit

Volatile organic compounds (VOCs) and Semi-Volatile Organic Compounds (SVOCs) arise from the chemicals used in the various stages of the leather manufacturing process. An important aim of the tanning industry is to minimize or eliminate VOCs and SVOCs, without lowering the quality of leather.   This paper shows the development of a new headspace-solid phase micro extraction coupled with gas chromatography–mass spectrometry (HS-SPME/GC-MS) method for the identification of VOCs and SVOCs emitted by newly designed polymers for the leather finishing operation. These new polymers are polyurethane resins designed to reduce the VOC and SVOC concentration. This method enables a simple and fast determination of the qualitative and semi-quantitative content of VOCs and SVOCs in polyurethane-type finishing resins. The chemicals that are of concern in this paper are the following: Dipropylene glycol Monomethyl Ether (DPGME), DBE-3 (a mixture of dibasic esters) and Triethylamine (TEA). The test conditions that have been determined to carry out the HS-SPME assay are the following: incubation time (2 hours), extraction temperature and time (40°C; 5 minutes) and the desorption conditions (280°C, 50 seconds).  Ten samples of laboratory scale resins were tested by HS-SPME followed by gas chromatography (GC-MS). DPGME and DBE-3 (a mixture of dimethyl adipate, dimethyl glutarate and dimethyl succinate) have been identified effectively. The compounds are identified by a quantitative method using external calibration curves for the target compounds. The technique is not effective to determine the TEA compound, since the chromatograms shown poor resolution peaks for the standard. 


2020 ◽  
Author(s):  
Hua-Ying Wang ◽  
Wei Zhang ◽  
Jian-Hua Dong ◽  
Hao Wu ◽  
Yuan-Hong Wang ◽  
...  

Abstract The floral scent of plants plays a key role in plant reproduction through the communication between plants and pollinators. Aquilegia as a model species for studying evolution, however, there have been few studies on the floral scents and relationships between floral scents and pollination for Aquilegia taxa. In this study, three types of solid-phase micro-extraction (SPME) fiber coatings (DVB/PDMS, CAR/PDMS, DVB/CAR/PDMS) were evaluated for their performance in extracting volatile organic compounds (VOCs) from flowers of Aquilegia amurensis, which can to contribute to the future studies of elucidating the role of floral scents in the pollination process. In total, 55 VOCs were identified, and among them, 50, 47 and 45 VOCs were extracted by the DVB/CAR/PDMS fiber, CAR/PDMS fiber and DVB/PDMS fibers, respectively. Only 30 VOCs were detected in A. japonica taxa. Furthermore, the relative contents of 8 VOCs were significant different (VIP > 1 and p < 0.05) between the A. amurensis and A. japonica. Therefore, the results can be applied in new studies of the relationships between the chemical composition of floral scents and the processes of attraction of pollinator. It may provide new ideas for rapid evolution and frequent interspecific hybridization of Aquilegia


2020 ◽  
Vol 14 (2) ◽  
pp. 61
Author(s):  
Rozita Osman

Headspace solid phase microextraction (HS-SPME) was employed for the extraction of volatile organic compounds (VOCs) in MD2 pineapple (Ananas comosus L. var. comosus cv. MD2). Optimisation of HS-SPME operating parameters was conducted using three-factor, three-level Box–Behnken response surface experimental design to evaluate the interactive effects of temperature (30 – 50 ºC), extraction time (10 – 30 min) and salting effect (1 – 3 g of salt addition) on the amount of selected VOCs. Determination of VOCs was done using gas chromatography with spectrometry detector (GC-MSD). Extraction temperature was found to be significant (p < 0.05) in increasing the amount of selected VOCs (ethyl acetate, methyl isobutyrate and butanoic acid methyl ester). Based on the maximum amount of these VOCs, the optimum operating extraction conditions for HS-SPME were set up at temperature of 30 °C, time of 29 min and salt addition of 1 g. The optimized HS-SPME conditions were employed for the extraction of VOCs from pineapple of different varieties.


BMC Chemistry ◽  
2021 ◽  
Vol 15 (1) ◽  
Author(s):  
Hua-Ying Wang ◽  
Wei Zhang ◽  
Jian-Hua Dong ◽  
Hao Wu ◽  
Yuan-Hong Wang ◽  
...  

Abstract Background The floral scents of plants play a key role in plant reproduction through the communication between plants and pollinators. Aquilegia as a model species for studying evolution, however, there have been few studies on the floral scents and relationships between floral scents and pollination for Aquilegia taxa. Methods In this study, three types of solid-phase micro-extraction (SPME) fiber coatings (DVB/PDMS, CAR/PDMS, DVB/CAR/PDMS) were evaluated for their performance in extracting volatile organic compounds (VOCs) from flowers of Aquilegia amurensis, which can contribute to the future studies of elucidating the role of floral scents in the pollination process. Results In total, 55 VOCs were identified, and among them, 50, 47 and 45 VOCs were extracted by the DVB/CAR/PDMS fiber, CAR/PDMS fiber and DVB/PDMS fibers, respectively. Only 30 VOCs were detected in A. japonica taxa. Furthermore, the relative contents of 8 VOCs were significant different (VIP > 1 and p < 0.05) between the A. amurensis and A. japonica. Conclusions The results can be applied in new studies of the relationships between the chemical composition of floral scents and the processes of attraction of pollinator. It may provide new ideas for rapid evolution and frequent interspecific hybridization of Aquilegia.


2020 ◽  
Vol 9 (7) ◽  
pp. e919974893
Author(s):  
Bárbara Oliveira Santos ◽  
Rodinei Augusti ◽  
Júlio Onésio Ferreira Melo ◽  
Jacqueline Aparecida Takahashi ◽  
Raquel Linhares Bello de Araújo

The pequi is a native specie from the Brazilian Cerrado that has great economic importance for the population of the region. The pericarp is considered an agroindustrial residue despite corresponding to approximately 80% of the total fruit mass. Informations about the chemical composition of pericarp would allow better utilization of this portion of the fruit. The objective of this study was to identify the best conditions of agitation, extraction time and extraction temperature to maximize the extraction of volatile organic compounds present in pequi pericarp (Caryocar brasiliense Camb.) using two types of solid phase microextraction fibers. The extraction of the volatile compounds was using the headspace solid-phase microextraction method with subsequent separation and identification by CG-MS. Polydimethylsiloxane/divinylbenzene (PDMS/DVB) fiber was statistically more efficient than divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber. The both fibers enabled the extraction and identification of 35 compounds, mainly terpenes (65.71%) and esters (14.29%). An increase in the extraction temperature and time allowed greater extraction of volatile compounds by both fibers. However, in relation to agitation, the best condition for using DVB/CAR/PDMS was 100 rpm, while agitation was not necessary for an efficient extraction using the PDMS/DVB fiber.


Molecules ◽  
2021 ◽  
Vol 26 (23) ◽  
pp. 7409
Author(s):  
Iva Šikuten ◽  
Petra Štambuk ◽  
Jasminka Karoglan Kontić ◽  
Edi Maletić ◽  
Ivana Tomaz ◽  
...  

(1) Background: Solid phase microextraction (SPME)-Arrow is a new extraction technology recently employed in the analysis of volatiles in food materials. Grape volatile organic compounds (VOC) have a crucial role in the winemaking industry due to their sensory characteristics of wine.; (2) Methods: Box–Behnken experimental design and response surface methodology were used to optimise SPME-Arrow conditions (extraction temperature, incubation time, exposure time, desorption time). Analyzed VOCs were free VOCs directly from grape skins and bound VOCs released from grape skins by acid hydrolysis.; (3) Results: The most significant factors were extraction temperature and exposure time for both free and bound VOCs. For both factors, an increase in their values positively affected the extraction efficiency for almost all classes of VOCs. For free VOCs, the optimum extraction conditions are: extraction temperature 60 °C, incubation time 20 min, exposure time 49 min, and desorption time 7 min, while for the bound VOCs are: extraction temperature 60 °C, incubation time 20 min, exposure time 60 min, desorption time 7 min.; (4) Conclusions: Application of the optimized method provides a powerful tool in the analysis of major classes of volatile organic compounds from grape skins, which can be applied to a large number of samples.


Separations ◽  
2020 ◽  
Vol 7 (4) ◽  
pp. 75
Author(s):  
Natalia Manousi ◽  
Erwin Rosenberg ◽  
George A. Zachariadis

A novel sample preparation method based on the use of the Arrow solid-phase microextraction device was used to extract and preconcentrate volatile organic compounds (VOCs) from milk samples prior to their determination by gas chromatography–mass spectrometry (GC-MS). The experimental parameters of the solid-phase microextraction (SPME) Arrow method were evaluated in terms of fiber type, sample volume, extraction temperature, extraction time, stirring rate and salt addition. Under the optimum extraction conditions, the SPME Arrow was compared with conventional SPME fibers to evaluate the effectiveness of the SPME Arrow method. Evaluation of the conventional SPME procedure was also performed under optimized conditions, for appropriate method comparison. Due to the larger sorption phase volume of SPME Arrow, a higher sensitivity and reproducibility were observed for the determined chromatographic peaks in comparison with conventional SPME fibers. The use of Carbon wide range (WR) SPME Arrow/polydimethylsiloxane (CAR/PDMS) SPME Arrow fibers leads to a compound-dependent improvement of a factor of 4–5x over the classical SPME setup. Moreover, the relative standard deviation (RSD) of the total volatiles for a conventional SPME procedure was 12.5%, while for SPME Arrow it was 6.2%. Finally, the novel method was successfully employed for the analysis of commercially available milk samples. The findings of this study indicate that SPME Arrow can be effectively used for the determination of volatile organic compounds in complex food matrixes.


2003 ◽  
Vol 3 (1) ◽  
pp. 769-796 ◽  
Author(s):  
A. C. Rivett ◽  
D. Martin ◽  
D. J. Gray ◽  
C. S. Price ◽  
G. Nickless ◽  
...  

Abstract. The results of a field campaign carried out from early spring through to the late summer of 2000, in Bristol, England, are presented. Continuous measurements of over 40 hydrocarbons have been made at an urban background site, located at Bristol University, for approximately nine months using a GC-FID system and for a selection of halocarbons for approximately one month using a GC-ECD system. In this paper we present the time-series of the nine halocarbons and selected hydrocarbons. Daytime and night-time hydroxyl radical concentrations have been estimated based on the diurnal variations of a selection of the measured hydrocarbons. The average summer daytime concentration of OH was found to be 2.5×106 molecules cm−3 and the night-time concentration to be in the range 104 to 105 molecules cm−3. In addition, the role played by certain VOCs in the formation of ozone is assessed using the POCP (Photochemical Ozone Creation Potential) concept.


2020 ◽  
Vol 16 (4) ◽  
pp. 404-412 ◽  
Author(s):  
Ihab Alnajim ◽  
Manjree Agarwal ◽  
Tao Liu ◽  
YongLin Ren

Background: The red flour beetle, Tribolium castaneum (Herbst) (Coleoptera: Tenebrionidae) is one of the world’s most serious stored grain insect pests. A method of early and rapid identification of red flour beetle in stored products is urgently required to improve control options. Specific chemical signals identified as Volatile Organic Compounds (VOCs) that are released by the beetle can serve as biomarkers. Methods: The Headspace Solid Phase Microextraction (HS-SPME) technique and the analytical conditions with GC and GCMS were optimised and validated for the determination of VOCs released from T. castaneum. Results: The 50/30 μm DVB/CAR/PDMS SPME fibre was selected for extraction of VOCs from T. castaneum. The efficiency of extraction of VOCs was significantly affected by the extraction time, temperature, insect density and type of SPME fibre. Twenty-three VOCs were extracted from insects in 4 mL flask at 35 ± 1°C for four hours of extraction and separated and identified with gas chromatography-mass spectroscopy. The major VOCs or chemical signals from T. castaneum were 1-pentadecene, p-Benzoquinone, 2-methyl- and p-Benzoquinone, 2-ethyl. Conclusion: This study showed that HS-SPME GC technology is a robust and cost-effective method for extraction and identification of the unique VOCs produced by T. castaneum. Therefore, this technology could lead to a new approach in the timely detection of T. castaneum and its subsequent treatment.


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