scholarly journals Extraction and Identification of a Wide Range of Microplastic Polymers in Soil and Compost

Polymers ◽  
2021 ◽  
Vol 13 (23) ◽  
pp. 4069
Author(s):  
Franja Prosenc ◽  
Pia Leban ◽  
Urška Šunta ◽  
Mojca Bavcon Kralj

Microplastic pollution is globally widespread; however, the presence of microplastics in soil systems is poorly understood, due to the complexity of soils and a lack of standardised extraction methods. Two commonly used extraction methods were optimised and compared for the extraction of low-density (polyethylene (PE)) and high-density microplastics (polyethylene (PET)), olive-oil-based extraction, and density separation with zinc chloride (ZnCl2). Comparable recoveries in a low-organic-matter matrix (soil; most >98%) were observed, but in a high-organic-matter matrix (compost), density separation yielded higher recoveries (98 ± 4% vs. 80 ± 11%). Density separation was further tested for the extraction of five microplastic polymers spiked at different concentrations. Recoveries were >93% for both soil and compost, with no differences between matrices and individual polymers. Reduction in levels of organic matter in compost was tested before and after extraction, as well as combined. Double oxidation (Fenton’s reagent and 1 M NaOH) exhibited the highest reduction in organic matter. Extracted microplastic polymers were further identified via headspace solid-phase microextraction–gas chromatography–mass spectrometry (HS-SPME–GC–MS). This method has shown the potential for descriptive quantification of microplastic polymers. A linear relationship between the number of particles and the signal response was demonstrated for PET, polystyrene (PS), polyvinyl chloride (PVC), and PE (R2 > 0.98 in alluvial soil, and R2 > 0.80 in compost). The extraction and identification methods were demonstrated on an environmental sample of municipal biowaste compost, with the recovery of 36 ± 9 microplastic particles per 10 g of compost, and the detection of PS and PP.

2000 ◽  
Vol 35 (2) ◽  
pp. 245-262 ◽  
Author(s):  
Francis I. Onuska ◽  
Ken A. Terry ◽  
R. James Maguire

Abstract The analysis of aromatic amines, particularly benzidines, at trace levels in environmental media has been difficult because of the lack of suitable deactivated capillary column stationary phases for gas chromatography. This report describes the use of an improved type of column as well as a method for the analysis of anilines and benzidines in water, wastewater and sewage samples. Extraction procedures are applicable to a wide range of compounds that are effectively partitioned from an aqueous matrix into methylene chloride, or onto a solid-phase extraction cartridge. The extracted analytes are also amenable to separation on a capillary gas chromatographic column and transferable to the mass spectrometer. These contaminants are converted to their N-trifluoroacetyl derivatives. Aniline and some substituted anilines, and 3,3’-dichlorobenzidine and benzidine were determined in 24-h composite industrial water, wastewater, primary sludge and final effluent samples at concentrations from 0.03 up to 2760 µg/L.


2004 ◽  
Vol 380 (2) ◽  
pp. 541-548 ◽  
Author(s):  
Hai-Shu LIN ◽  
Andrew M. JENNER ◽  
Choon Nam ONG ◽  
Shan Hong HUANG ◽  
Matthew WHITEMAN ◽  
...  

8-Hydroxy-2´-deoxyguanosine (8OHdG) is a widely used biomarker for the measurement of endogenous oxidative DNA damage. A sensitive method for the quantification of 8OHdG in urine by single solid-phase extraction and GC-MS (gas chromatography with MS detection) using selective ion monitoring is described in the present study. After solid-phase extraction, samples are freeze-dried, derivatized by trimethylsilylation and analysed by GC-MS. The urinary 8OHdG was quantified using heavy isotope dilution with [18O]8OHdG. The recovery of 8OHdG after the solid-phase extraction ranged from 70 to 80% for a wide range of urinary 8OHdG levels. Using 1 ml of urine, the limit of quantification was >2.5 nM (2.5 pmol/ml) and the calibration curve was linear in the range 2.5–200 nM. This method was applied to measure 8OHdG in urine samples from 12 healthy subjects. The intra- and inter-day variations were <9%. Urinary 8OHdG levels in spot urine samples from four healthy subjects were also measured for 1 week and, again, the variation was small. The presence of H2O2 in urine did not cause artifactual formation of 8OHdG. Since this assay is simple, rapid, sensitive and reproducible, it seems suitable to be used as a routine methodology for the measurement of urinary excretion of 8OHdG in large population studies.


2018 ◽  
Vol 8 (1) ◽  
Author(s):  
A.G.W.U. Perera ◽  
M.M.S.C. Karunaratne ◽  
S.D.M. Chinthaka

Neem (Azadirachta indica A. juss), is known to possess a wide range of pharmacological properties and is thus commercially exploitable. Apart from its medicinal potential, a considerable progress has been achieved regarding biological potential and chemical composition of the leaves which is an ever-increasing interest to the scientific community. During this study, biological phenomena and secondary metabolite composition of A. indica leaves were examined in the management of Sitophilus zeamais on stored maize. Insecticidal and repellent potential of A. indica leaf powders were evaluated in both contact and fumigant forms. Phytochemical screening of 11 phyto constituents was performed following the standard procedures for n-hexane, dichloromethane, ethyl acetate, methanol and aqueous leaf extracts. Volatile profile of A. indica leaves was characterized by employing headspace-solid-phase micro extraction coupled with gas chromatography-mass spectrometry (HS-SPME/GC-MS). Over 60% weevil repellency was recorded at doses above 23.33%, whereas 100% and 67% contact and fumigation mortalities were observed respectively, 9 days after treatment at the dose of 33.33% and the respected LD50 values were 1.56 g and 4.48 g. Thirty two volatile compounds were identified in three distinct chemical classes (Monoterpenoid, sesquiterpenoid and purine nucleosides). γ-Elemene (24.06%), 3,7 (11)-eudesmadiene (6.83%), caryophyllene (6.40%), and 10s,11s-himachala-3(12),4-diene (6.36%) were the major constituents of neem leaf volatiles, followed by other compounds present in less than 4% which might be responsible for varied biological activities observed. Thus the odour impact of the bioassayguided study clearly implies that A. indica leaves can be harnessed against S. zeamais infestations.Keywords: Azadirachta indica, Sitophilus zeamais, headspace-solid-phase micro-extraction, insecticidal activity, repellency


Molecules ◽  
2019 ◽  
Vol 24 (8) ◽  
pp. 1639 ◽  
Author(s):  
Liakh ◽  
Pakiet ◽  
Sledzinski ◽  
Mika

Oxylipins are potent lipid mediators derived from polyunsaturated fatty acids, which play important roles in various biological processes. Being important regulators and/or markers of a wide range of normal and pathological processes, oxylipins are becoming a popular subject of research; however, the low stability and often very low concentration of oxylipins in samples are a significant challenge for authors and continuous improvement is required in both the extraction and analysis techniques. In recent years, the study of oxylipins has been directly related to the development of new technological platforms based on mass spectrometry (LC–MS/MS and gas chromatography–mass spectrometry (GC–MS)/MS), as well as the improvement in methods for the extraction of oxylipins from biological samples. In this review, we systematize and compare information on sample preparation procedures, including solid-phase extraction, liquid–liquid extraction from different biological tissues.


Author(s):  
João Junqueira ◽  
Michelle do Nascimento ◽  
Lucas da Costa ◽  
Lincoln Romualdo ◽  
Francisco de Aquino ◽  
...  

Xylopia aromatica (Lam.) Mart. (Annonaceae) is a typical species from the Brazilian cerrado that presents medicinal properties. The plant is distinguished by its large white flowers which produce a pleasant fragrance. X. aromatica is characterized by a wide range of medicinal application. These characteristics have motivated us to investigate the flowers volatile organic compounds (VOCs) via in vivo and in vitro protocols by a headspace solid-phase microextraction (HS‑SPME) technique combined with gas chromatography-mass spectrometry (HS-SPME/GC‑MS). Four different fibers, extraction times and temperatures were the parameters changed to lead to the maximum profiling of the volatile constituents. Data were analyzed using principal component analysis (PCA). A total of 77 VOCs were extracted from the floral scent, with 52 and 68 extracted from in vivo and in vitro sampling, respectively, of which 48 were reported for the first time in the literature as volatile constituents from X. aromatica flowers. The extraction and identification of VOCs were successfully performed through HS-SPME/GC-MS. The PCA data allowed the identification of parameters that led to the maximum number of VOCs, which were polyacrylate (PA) and carboxen/polydimethylsiloxane (CAR/PDMS) fibers, 60 min extraction time and temperature of 29.0 °C. Among the volatile constituents identified, sesquiterpenes predominated, comprising about 61.04%.


Foods ◽  
2019 ◽  
Vol 8 (9) ◽  
pp. 415 ◽  
Author(s):  
Kung ◽  
Chen ◽  
Chao ◽  
Wu ◽  
Lin ◽  
...  

Hsian-tsao (Platostoma palustre Blume) is a traditional Taiwanese food. It is admired by many consumers, especially in summer, because of its aroma and taste. This study reports the analysis of the volatile components present in eight varieties of Hsian-tsao using headspace solid-phase microextraction (HS-SPME) and simultaneous distillation-extraction (SDE) coupled with gas chromatography (GC) and gas chromatography-mass spectrometry (GC/MS). HS-SPME is a non-heating method, and the results show relatively true values of the samples during flavor isolation. However, it is a kind of headspace analysis that has the disadvantage of a lower detection ability to relatively higher molecular weight compounds; also, the data are not quantitative, but instead are used for comparison. The SDE method uses distillation 2 h for flavor isolation; therefore, it quantitatively identifies more volatile compounds in the samples while the samples withstand heating. Both methods were used in this study to investigate information about the samples. The results showed that Nongshi No. 1 had the highest total quantity of volatile components using HS-SPME, whereas SDE indicated that Taoyuan Mesona 1301 (TYM1301) had the highest volatile concentration. Using the two extraction methods, 120 volatile components were identified. Fifty-six volatile components were identified using HS-SPME, and the main volatile compounds were α-pinene, β-pinene, and limonene. A total of 108 volatile components were identified using SDE, and the main volatile compounds were α-bisabolol, β-caryophyllene, and caryophyllene oxide. Compared with SDE, HS-SPME sampling extracted a significantly higher amount of monoterpenes and had a poorer detection of less volatile compounds, such as sesquiterpenes, terpene alcohols, and terpene oxide.


2003 ◽  
Vol 86 (2) ◽  
pp. 412-431 ◽  
Author(s):  
Michelangelo Anastassiades ◽  
Steven J Lehotay ◽  
Darinka Štajnbaher ◽  
Frank J Schenck

Abstract A simple, fast, and inexpensive method for the determination of pesticide residues in fruits and vegetables is introduced. The procedure involves initial single-phase extraction of 10 g sample with 10 mL acetonitrile, followed by liquid–liquid partitioning formed by addition of 4 g anhydrous MgSO4 plus 1 g NaCl. Removal of residual water and cleanup are performed simultaneously by using a rapid procedure called dispersive solid-phase extraction (dispersive-SPE), in which 150 mg anhydrous MgSO4 and 25 mg primary secondary amine (PSA) sorbent are simply mixed with 1 mL acetonitrile extract. The dispersive-SPE with PSA effectively removes many polar matrix components, such as organic acids, certain polar pigments, and sugars, to some extent from the food extracts. Gas chromatography/mass spectrometry (GC/MS) is then used for quantitative and confirmatory analysis of GC-amenable pesticides. Recoveries between 85 and 101% (mostly &gt;95%) and repeatabilities typically &lt;5% have been achieved for a wide range of fortified pesticides, including very polar and basic compounds such as methamidophos, acephate, omethoate, imazalil, and thiabendazole. Using this method, a single chemist can prepare a batch of 6 previously chopped samples in &lt;30 min with approximately $1 (U.S.) of materials per sample.


Separations ◽  
2018 ◽  
Vol 5 (3) ◽  
pp. 45 ◽  
Author(s):  
Kevin Eckert ◽  
David Carter ◽  
Katelynn Perrault

Volatile organic compounds (VOCs) are monitored in numerous fields using several commercially-available sampling options. Sorbent-based sampling techniques, such as solid-phase microextraction (SPME), provide pre-concentration and focusing of VOCs prior to gas chromatography–mass spectrometry (GC–MS) analysis. This study investigated the dynamics of SPME Arrow, which exhibits an increased sorbent phase volume and improved durability compared to traditional SPME fibers. A volatile reference mixture (VRM) and saturated alkanes mix (SAM) were used to investigate optimal parameters for microbiological VOC profiling in combination with GC–MS analysis. Fiber type, extraction time, desorption time, carryover, and reproducibility were characterized, in addition to a comparison with traditional SPME fibers. The developed method was then applied to longitudinal monitoring of Bacillus subtilis cultures, which represents a ubiquitous microbe in medical, forensic, and agricultural applications. The carbon wide range/polydimethylsiloxane (CWR/PDMS) fiber was found to be optimal for the range of expected VOCs in microbiological profiling, and a statistically significant increase in the majority of VOCs monitored was observed. B. subtilis cultures released a total of 25 VOCs of interest, across three different temporal trend categories (produced, consumed, and equilibrated). This work will assist in providing foundational data for the use of SPME Arrow in future microbiological applications.


Foods ◽  
2020 ◽  
Vol 9 (10) ◽  
pp. 1422
Author(s):  
Jiyoon Cha ◽  
Young-Wook Chin ◽  
Jun-Young Lee ◽  
Tae-Wan Kim ◽  
Hae Won Jang

The SPME Arrow technology—a novel solid phase micro-extraction technique—was used to analyze Soju, a traditional Korean distilled liquor, in barrels made of Quercus spp. The volatile compounds detected when the barrels were toasted were analyzed. Five types of sorbents—carbon wide range/polydimethylsiloxane, divinylbenzene/carbon wide range/polydimethylsiloxane, divinylbenzene/polydimethylsiloxane, polydimethylsiloxane, and polyacrylate—were used for this investigation. Fifty-four volatile compounds were detected in Soju using gas chromatography/mass spectrometry. A high extraction efficiency was obtained using carbon wide range/polydimethylsiloxane. Nineteen samples were analyzed using barrels made of six species of carbonated oak (Q. aliena, Q. variabilis, Q. dentate, Q. acutissima, Q. mongolica, and Q. serrata) and control groups in three ways: noncharring, medium charring, and heavy charring. Ethanol, 1-propanol, isoamyl acetate, and isoamyl alcohol can be used as indicator volatile components for Soju and other such traditional Korean distilled liquors. We believe our study results can be used to design better analysis methods for Soju and other distilled liquors.


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