Solid-phase microextraction (SPME) for determination of geosmin and 2-methylisoborneol in volatile emissions from soil disturbance

2021 ◽  
Author(s):  
Morgan Conrady ◽  
Markus Bauer ◽  
Kyoo Jo ◽  
Donald Cropek ◽  
Ryan Busby

A method is described here for the concentration and determination of geosmin and 2-methylisoborneol (2-MIB) from the gaseous phase, with translation to field collection and quantification from soil disturbances in situ. The method is based on the use of solid-phase microextraction (SPME) fibers for adsorption of volatile chemicals from the vapor phase, followed by desorption into a gas chromatograph-mass spectrometer (GC-MS) for analysis. The use of a SPME fiber allows simple introduction to the GC-MS without further sample preparation. Several fiber sorbent types were studied and the 50/30 μm DVB/CAR/PDMS was the best performer to maximize the detected peak areas of both analytes combined. Factors such as extraction temperature and time along with desorption temperature and time were explored with respect to analyte recovery. An extraction temperature of 30 ◦C for 10 min, with a desorption temperature of 230 ◦C for 4 min was best for the simultaneous analysis of both geosmin and 2-MIB without complete loss of either one. The developed method was used successfully to measure geosmin and 2-MIB emission from just above disturbed and undisturbed soils, indicating that this method detects both compounds readily from atmospheric samples. Both geosmin and 2-MIB were present as background concentrations in the open air, while disturbed soils emitted much higher concentrations of both compounds. Surprisingly, 2-MIB was always detected at higher concentrations than geosmin, indicating that a focus on its detection may be more useful for soil emission monitoring and more sensitive to low levels of soil disturbance.

2002 ◽  
Vol 85 (6) ◽  
pp. 1205-1209 ◽  
Author(s):  
Kamal Ayoub ◽  
Leonard Harris ◽  
Bill Thompson

Abstract Current methods of analysis for ethylene oxide (EO) in medical devices include headspace and simulated-use extractions followed by gas chromatography with either a packed or a capillary column. The quantitation limits are about 0.5–1.0 μg/g for a packed column and about 0.1–0.2 μg/g for a capillary column. The current allowable levels of EO on medical devices sterilized with EO gas as outlined in International Organization for Standardization (ISO) 10993-7 may be significantly reduced from current levels by applying the ISO Draft International Standard 10993-17 method for establishing allowable limits. This may require EO test methods with detection and quantitation limits that are much lower than those of the currently available methods. This paper describes a new method that was developed for the determination of low-level EO by solid-phase microextraction using the direct-immersion method. Factors such as temperature and stirring were found to affect absorption efficiency and absorption time. A low extraction temperature (about 6°C) was found to be more efficient than room-temperature extraction. Stirring was found to reduce absorption time by about 50%. Under these conditions, detection and quantitation limits of 0.002 and 0.009 μg/g, respectively, were obtained by using a capillary column. As a result, this method makes compliance with lower EO limits feasible.


2013 ◽  
Vol 96 (6) ◽  
pp. 1430-1434 ◽  
Author(s):  
Maurizio Boccacci Mariani ◽  
Vanessa Giannetti ◽  
Elena Testani ◽  
Valentina Ceccarelli

Abstract The use of pesticides in agriculture has grown dramatically over the last decades. Environmental exposure of humans to agrochemicals is common and results in both acute and chronic health effects. In this study, direct immersion-solid phase microextraction (SPME) was coupled with electron capture detection for trace determination of 19 chlorinated pesticides in tomato samples, using a 100 μm polydimethylsiloxane fiber. The experimental parameters extraction time, extraction temperature, stirring, and salting out were evaluated and optimized. The LODs ranged from 0.5 to 8 μg/kg, and the LOQs from 5 to 30 μg/kg. A linear response was confirmed by correlation coefficients ranging from 0.97 to 0.9985. The developed method was tested by analyzing real samples purchased within the network of Italian distribution. The samples were found to be free from detectable residues of the studied pesticides. SPME has been shown to be a fast extraction technique that has several advantages such as solvent-free extraction, simplicity, and compatibility with the chromatographic analytical system.


2017 ◽  
Vol 100 (1) ◽  
pp. 218-223 ◽  
Author(s):  
Nasim Mohammadnezhad ◽  
Amir Abbas Matin ◽  
Naser Samadi ◽  
Ashkan Shomali ◽  
Hassan Valizadeh

Abstract Linear ionic liquid bonded to fused silica and its application as a solid-phase microextraction fiber for the extraction of bisphenol A (BPA) from water samples were studied. Afteroptimization of microextraction conditions (15 mL sample volume, extraction time of 40 min, extraction temperature of 30± 1°C, 300 μL acetonitrile as the desorption solvent, and desorption time of 7 min), the fiber was used to extract BPA from packed mineral water, followed by HPLC–UV on an XDB-C18 column (150 × 4.6 mm id, 3.5 μm particle) with a mobile phase of acetonitrile–water (45 + 55%, v/v) and flow rate of 1 mL . min−1). A low LOD (0.20 μg. L−1) and good linearity (0.9977) in the calibration graph indicated that the proposed method was suitable for the determination of BPA.


2014 ◽  
Vol 881-883 ◽  
pp. 61-64
Author(s):  
Zhao Xi Fang ◽  
Guo Qin Liu ◽  
Xue De Wang ◽  
Li Juan Han ◽  
Bing Ge Liu

This paper was to develop a simple and rapid headspace solid-phase microextraction (HS-SPME) method coupled with gas chromatography–mass spectrometry (GC-MS) for the determination of volatiles compounds from the roasted sesame oil (RSO). A HP-5MS capillary column (30 m × 0.25 mm I.D. × 0.25 mm film thick) was used for GC-MS, and a 50/30 μm divinylbenzene/carboxen/polydimethylsiloxane (DVB/CAR/PDMS) fiber was used to extract volatiles compounds. The condition was optimized by varying the sample-to-headspace ratio (0.5-2.5 g/15 ml), extraction time (10-50 min) and Splitless time (0.5-4 min). The results showed that the optimal operating conditions occurred at (extraction temperature:40°C, sample-to-headspace ratio: 1.5 g/15 ml, extraction time: 40 min, Splitless time: 1 min) for the analyze method.


Author(s):  
Ying PENG ◽  
Huan HE ◽  
Cheng SUN ◽  
Ya-Ling ZHANG ◽  
Wen-Chao LI ◽  
...  

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