Gas Chromatography-flame Photometric Detection Research Articles

Speciation of butyl and phenyltin compounds using dispersive liquid–liquid microextraction and gas chromatography-flame photometric detection

Dispersive liquid–liquid microextraction and gas chromatography-flame photometric detection (DLLME-GC-FPD) were performed for the speciation of butyl and phenyltin compounds in water samples after derivatization with sodium tetraethylborate (NaBEt 4). Some important parameters, such as pH, amount of NaBEt 4, derivatization time, kind and volume of extraction and disperser solvents, extraction time and salt effect were investigated and optimized. High enrichment factors (825–1036) and low detection limits (0.2–1 ng L −1) were obtained under the optimum conditions. The calibration graphs were linear in the range of 0.5–1000 ng L −1 (as Sn) for the target analytes. The relative standard deviations (RSDs) for the extraction of 20 ng L −1 (as Sn) of butyl and phenyltin compounds varied from 2.3 to 5.9% ( n = 7) and from 4.1 to 8.8% ( n = 7) with and without using internal standard, respectively. Seawater and river water samples were successfully analyzed using the proposed method and the relative recoveries of the studied compounds in the water samples, at spiking levels of 10.0 and 100 ng L −1 (as Sn) were obtained to be 82.5–104.7%.

Comparison of hollow fiber liquid phase microextraction and dispersive liquid–liquid microextraction for the determination of organosulfur pesticides in environmental and beverage samples by gas chromatography with flame photometric detection

Two methods based on hollow fiber liquid phase microextraction (HF-LPME) and dispersive liquid–liquid microextraction (DLLME), have been critically compared for the analysis of organosulfur pesticides (OSPs) in environmental and beverage samples by gas chromatography-flame photometric detection (GC-FPD). Experimental conditions including extraction solvent, solvent volume, extraction time, temperature and ionic strength have been investigated for both HF-LPME and DLLME. Under the optimal conditions, the limits of detection for the six target OSPs (malathion, chlorpyrifos, buprofezin, triazophos, carbosulfan and pyridaben) obtained by HF-LPME–GC-FPD and DLLME–GC-FPD were ranged from 1.16 μg/L to 48.48 μg/L and 0.21 μg/L to 3.05 μg/L, respectively. The relative standard deviations (RSDs, n = 5) were in the range of 3.4–8.0% and 8.5–13.7%with the enrichment factors (EFs) of 27–530 and 176–946 folds for HF-LPME–GC-FPD and DLLME–GC-FPD, respectively. Both methods were found to be simple, fast, efficient, and inexpensive. Compared with HF-LPME, the advantages of DLLME technique were less extraction time, suitable for batches of samples pretreatment simultaneously, a higher extraction capacity when analyzing simple samples such as water samples. While for the analysis of complicated matrix samples such as soil and beverage samples, HF-LPME was demonstrated to be more robust and more suitable. Both methods were applied to the analysis of six OSPs in different waters, soil and beverage samples, and no target OSPs was found in these samples. For analysis of the spiked samples, the recovery of 81.7–114.4% with RSDs of 0.6–9.6% were obtained for HF-LPME, and the recovery of 78.5–117.2% with RSDs of 0.6–11.9% were obtained for DLLME.

Preliminary Studies of Sulphur Mustard–Induced Lung Injury in the Terminally Anesthetized Pig: Exposure System and Methodology

ABSTRACTAlthough normally regarded as a vesicant, inhalation of sulphur mustard (HD) vapor can cause life-threatening lung injury for which there is no specific treatment. Novel therapies for HD-induced lung injury are best investigated in an in vivo model that allows monitoring of a range of physiological variables.HD vapor was generated using two customized thermostatically controlled glass flasks in parallel. The vapor was passed into a carrier flow of air (81 L· min−1) and down a length of glass exposure tube (1.75 m). A pig was connected to the midpoint of the exposure tube via a polytetrafluoroethylene-lined endotracheal tube, Fleisch pneumotachograph, and sample port. HD vapor concentrations (40–122.8 mg. m−3) up-and downstream of the point of exposure were obtained by sampling onto Porapak absorption tubes with subsequent analysis by gas chromatography-flame photometric detection. Real-time estimates of vapor concentration were determined using a photo-ionization detector. Lung function indices (respiratory volumes, lung compliance, and airway resistance) were measured online throughout.Trial runs with methylsalicylate (MS) and animal exposures with HD demonstrated that the exposure system rapidly reached the desired concentration within 1 min and maintained stable output throughout exposure, and that the MS/HD concentration decayed rapidly to zero when switched off.A system is described that allows reproducible exposure of HD vapor to the lung of anesthetized white pigs. The system has proved to be robust and reliable and will be a valuable tool in assessing potential future therapies against HD-induced lung injury in the pig.Crown Copyright (c) 2007 Dstl.

Extraction and determination of organophosphorus pesticides in water samples by a new liquid phase microextraction–gas chromatography–flame photometric detection

A rapid, sensitive and efficient liquid phase microextraction (LPME) method was developed to determine trace concentrations of some organophosphorus pesticides in water samples. This method combines liquid phase microextraction with gas chromatographic (GC) analysis in a simple and inexpensive apparatus involving very little organic solvent consumption. It involves exposing a floated drop of an organic solvent on the surface of aqueous solution in a sealed vial. Experimental parameters which control the performance of LPME such as type of organic solvent, organic solvent and sample volumes, sample stirring rate, sample solution temperature, salt addition and exposure time were investigated and optimized. Finally, the enrichment factor, dynamic linear range (DLR), limit of detection (LOD) and precision of the method were evaluated by the water samples spiked with organophosphorus pesticides. Using optimum extraction conditions, very low detection limits (0.01–0.04 μg L −1) and good linearities (0.9983 < r 2 < 0.9999) were achieved. The LPME was performed for determination of organophosphorus pesticides in different types of natural water samples and acceptable recoveries (96–104%) and precisions (3.5 < R.S.D.% < 8.9) were obtained. The results suggested that the newly proposed LPME method is a rapid, accurate and effective sample preparation method and could be successfully applied for extraction and determination of organophosphorus pesticides in water samples.

Application of dispersive liquid–liquid microextraction for the analysis of organophosphorus pesticides in watermelon and cucumber

In this article, a new method for the determination of organophosphorus pesticides (OPPs) in cucumber and watermelon was developed by using dispersive liquid–liquid microextraction (DLLME) and gas chromatography–flame photometric detection (GC-FPD). Acetonitrile (MeCN) was used as extraction solvent for the extraction of OPPs from plant samples. When the extraction process was finished, the target analytes in the extraction solvent were rapidly transferred from the MeCN extract to another small volume of organic solvent, chlorobenzene, using DLLME. Recovery tests were performed for concentrations between 0.5 and 20 μg/kg; recoveries for each target analyte were in the range between 67 and 111%. The repeatability of the proposed method, expressed as relative standard deviation, varied between 2 and 9% ( n = 3). Limits of detection of the method for watermelon and cucumber were found ranging from 0.010 to 0.190 μg/kg for all the target pesticides. Compared with the conventional sample preparation method, the proposed method has the advantage of being quick and easy to operate, and having high-enrichment factors and low consumption of organic solvent.

Parameters affecting microwave-assisted extraction of organophosphorus pesticides from agricultural soil

This work describes an optimised method for the determination of six representative organophosphorus pesticides (OPPs) (diazinon, parathion, methyl pirimiphos, methyl parathion, ethoprophos, and fenitrothion) in agricultural soils. The method is based on microwave-assisted extraction using a water–methanol modified mixture for desorption and simultaneous partitioning on n-hexane (MAEP), together with gas chromatography–flame photometric detection (GC–FPD). To improve GC–FPD signals (peak intensity and shape) olive oil was used effectively as a “matrix mimic”. The optimisation of the extraction method was achieved in two steps: an initial approach through experimental design and principal component analysis where recovery of compounds using a water–methanol mixture ranged from 54 to 77%, and the second one by studying the addition of KH 2PO 4 to the extracting solution where recoveries were significantly increased, molecular replacing of OPPs from adsorption sites by phosphate being the probable extraction mechanism. Under optimised conditions, recoveries of pesticides from different soils were higher than 73%, except for methyl parathion in some soils, with SD equal or lower than 11% and detection limits ranging from 0.004 to 0.012 μg g −1. The proposed method was used to determine OPPs in soil samples from different agricultural zones of Chile.

Separation of dialkyl sulfides by metallomesogenic stationary phases for complexation gas chromatography

A copper mesogenic side-chain polymer (P-C 15CuC 18) was cross-linked onto the capillary wall as a stationary film for gas chromatography (GC) separation of alkylsulfides. These organic sulfides are of interest for their large health impact because of their wide range of volatilities and high reactivities toward metals. Different GC parameters for optimal separation efficiency are discussed for use with a mesogenic polymer column along with flame photometric detection (FPD). Both the carrier gas flow-rate and column temperature were studied to determine the relationship of plate height to the chemical structure of the solutes, as well as to determine the morphology of the mesogenic polymer. Van ’t Hoff plots show phase transitions of the stationary mesophase as the column temperature was varied. The results reveal that the separation mechanism might be based on ligand exchange and polarity interaction between the analytes and the stationary phase, with the vapor pressure of the analytes also being important. The former interaction dominates in the lamellar crystalline phase and the latter interaction dominates in the hexagonal columnar-discotic phase. With high reproducibility for retention time (RSD ≤ 0.37%) and for peak area (RSD ≤ 5.16%), the GC–FPD system produced linear calibration graphs ( r ≥ 0.9918) for the determination of 13 sulfides with a detection limit below 2.5 ng.

A one-year survey of organotin compounds in the reservoirs supplying the drinking water treatment plants of Athens, Greece

Organotin compounds belong to the priority list of substances regulated by 76/464/EEC Directive, as well as by 2000/60/EC Water Framework Directive, because they pose considerable risks to the environment and human health. They are the most commonly used organometallic compounds with estimated global amount produced 50,000 tons per year. Therefore, they have been detected worldwide in surface waters, drinking water, sediments and biota. The objective of the present investigation was the determination of these compounds in the water sources supplying the drinking water treatment plants of Athens, Greece, in particular at the reservoirs Mornos, Marathonas, Yliki and Evinos. The quality of water of those reservoirs could be affected from human activities, such as industry and agriculture, as well as from settlements in the area nearby. The surface water sampling campaigns executed were seasonal, during the period March 2004–May 2005, while finished drinking water samples from the distribution network of Athens were also analyzed. Six organotin species (monobutyltin, dibutyltin, tributyltin, monophenyltin, diphenyltin and triphenyltin) were determined by a gas chromatography — flame photometric detector (GC-FPD) method, after sample pretreatment with simultaneous liquid–liquid extraction with hexane and derivatization with tetraethyl borate. The results showed that the waters studied are free from organotin compounds, except for a limited number of samples, where the occurrence of some organotin species at low concentrations was observed.

Methylation mechanism of tin(II) by methylcobalamin in aquatic systems

The methylation reaction of tin(II) with methylcobalamin (CH(3)B(12)) in aquatic systems was modeled in the laboratory. The products were detected by a sensitive gas chromatography-flame photometric detector (GC-FPD), and further identified by gas chromatography-mass spectrometry (GC-MS). Both monomethyltin (MMT) and dimethyltin (DMT) were found as methylation products. Three important effecting factors during the methylation reaction, salinity, pH and aerobic or anaerobic, were studied. The results showed that methyl group can be transferred from CH(3)B(12) to tin in aquatic solutions as a radical or carbonium, as well as a carbanion. Two explanations for the pH-dependency of the methylation reaction between tin(II) and CH(3)B(12) were proposed: pH-dependency of the equilibrium states of CH(3)B(12), and pH-dependency of inorganic tin(II) species whose reactivity vary with the redox potential in the solution. Salinity can influence the activity of the methyl donor, which cause changes in the methylation efficiency. Kinetic experiments showed that the methylation reaction was pseudo-first-order for CH(3)B(12).

Identification of compounds associated with testosterone depressions in fish exposed to bleached kraft pulp and paper mill chemical recovery condensates

In previous experiments, bleached kraft chemical recovery condensates generated during softwood pulp production have been identified as a primary source of substances causing testosterone depressions in mummichog (Fundulus heteroclitus). Recent toxicity identification evaluations have encountered inconsistencies in the potential of condensates and fractions to reduce steroid concentrations between three repeated exposures. To assess the sources of these inconsistencies, temporal assessments of condensate extractives and analytical methodologies were evaluated. Condensates were collected during a six-month period, extracted by solid-phase extraction (SPE), and analyzed by gas chromatography-mass spectrometry and gas chromatography-flame photometric detection. All unique extractives were cataloged by mass spectra, peak area, and gas chromatographic retention time, and nine were confirmed and quantified against authentic standards. Confirmed components included phenolic guaiacyl-based lignin degradation products, sulfur (S9), three diterpenoids, and a dimethoxy stilbene. Concentrations of confirmed condensate extractives were consistent in all samples collected. Spiking experiments of confirmed extractives revealed substantial losses following high-pressure liquid chromatographic fractionation and three different methods of fraction preparation. In an effort to propose chemical classes associated with biological activity, all unique condensate extractives in previously established bioactive and inactive fractions were classified based on their potential to depress testosterone in mummichog. Of 39 unique components in bioactive SPE extracts of condensates, six were associated with hormonal activity. Mass spectral interpretation indicated hydroxylated diterpenoids, sesquiterpenoids, and a lignin-derived stilbene as classes of chemicals associated with steroid depressions.

Dispersive liquid–liquid microextraction combined with gas chromatography-flame photometric detection: Very simple, rapid and sensitive method for the determination of organophosphorus pesticides in water

A new method was used for the extraction of organophosphorus pesticides (OPPs) from water samples: dispersive liquid–liquid microextraction (DLLME) coupled with gas chromatography-flame photometric detection (GC-FPD). In this extraction method, a mixture of 12.0 μL chlorobenzene (extraction solvent) and 1.00 mL acetone (disperser solvent) is rapidly injected into the 5.00 mL water sample by syringe. Thereby, a cloudy solution is formed. In fact, the cloudy state is because of the formation of fine droplets of chlorobenzene, which has been dispersed among the sample solution. In this step, the OPPs in water sample are extracted into the fine droplets of chlorobenzene. After centrifuging (2 min at 5000 rpm), the fine droplets of chlorobenzene are sedimented in the bottom of the conical test tube (5.0 ± 0.3 μL). Sedimented phase (0.50 μl) is injected into the GC for separation and determination of OPPs. Some important parameters, such as kind of extraction and disperser solvent and volume of them, extraction time, temperature and salt effect were investigated. Under the optimum conditions, the enrichment factors and extraction recoveries were high and ranged between 789–1070 and 78.9–107%, respectively. The linear range was wide (10–100 000 pg/mL, four orders of magnitude) and limit of detections were very low and were between 3 to 20 pg/mL for most of the analytes. The relative standard deviations (RSDs) for 2.00 μg/L of OPPs in water with internal standard were in the range of 1.2–5.6% ( n = 5) and without internal standard were in the range of 4.6–6.5%. The relative recoveries of OPPs from river, well and farm water at spiking levels of 50, 500 and 5000 pg/mL were 84–125, 88–123 and 93–118%, respectively. The performance of proposed method was compared with solid-phase microextraction (SPME) and single drop microextraction. DLLME is a very simple and rapid (less than 3 min) method, which requires low volume of sample (5 mL). It also has high enrichment factor and recoveries for extraction of OPPs from water.

Vinyl crown ether as a novel radical crosslinked sol–gel SPME fiber for determination of organophosphorus pesticides in food samples

A method based on solid-phase microextraction and gas chromatography flame photometric detector for the determination of organophosphorus pesticides (OPPs) in food samples was described. Three kinds of vinyl crown ether polar fibers were prepared with sol–gel process and used for the analytes. The new coatings showed higher extraction efficiency and sensitivity for organophosphorus pesticides compared with commercial fibers—85 μm PA and 65 μm PDMS-DVB. Specifically, the benzo-15-crown-5 coating was the most effective for the target analytes. Several factors affecting the performance of SPME such as extraction temperature and time, salt addition, and dilution ratios of samples were optimized. The apparent recoveries of spiked food samples (apple juice, apple and tomato) were determined to be over 55.3% and the limits of detection (LODs) were in the range of 0.003–0.09 ng/g for the OPP studied. The method was applied to determine the concentrations of OPP in real food samples.

Optimization of a single-drop microextraction procedure for the determination of organophosphorus pesticides in water and fruit juice with gas chromatography-flame photometric detection

A single-drop microextraction (SDME) procedure was developed for the analysis of organophosphorus pesticides (OPPs) in water and fruit juice by gas chromatography (GC) with flame photometric detection (GC-FPD). The significant parameters affecting the SDME performance such as selection of microextraction solvent, solvent volume, extraction time, stirring rate, sample pH and temperature, and ionic strength were studied and optimized. Two types of SDME mode, static and cycle-flow SDME, were evaluated. The static SDME procedure provided more sensitive analysis of the target analytes. Therefore, static SDME with tributyl phosphate (TBP) as internal standard was selected for the real sample analysis. The limits of detection (LODs) in water for the six studied compounds were between 0.21 and 0.56 ng/mL with the relative standard deviations ranging from 1.7 to 10.0%. Linear response data was obtained in the concentration range of 0.5–50 ng/mL (except for dichlorvos 1.0–50 ng/mL) with correlation coefficients from 0.9995 to 0.9999. Environmental water sample collected from East Lake and fruit juice samples were successfully analyzed using the proposed method, but none of the analytes in both lake water and fruit juice were detected. The recoveries for the spiked water and juice samples were from 77.7 to 113.6%. Compared with the conventional methods, the proposed method enabled a rapid and simple determination of organophosphorus pesticides in water and fruit juice with minimal solvent consumption and a higher concentration capability.

Determination of organophosphorus pesticides in water samples by single drop microextraction and gas chromatography-flame photometric detector

In this paper we have developed single drop microextraction (SDME) with modified 1.00 μl microsyringe, followed by gas chromatography with flame photometric detector (GC-FPD) for determination of 13 organophosphorus pesticides (OPPs) in water samples. By using a 1.00 μl microsyringe the repeatability of drop volume and injection were improved, because of using maximum volume of microsyringe and no dead volume. On the other hand, the modification of needle tip caused increasing cross section of needle tip and increasing adhesion force between needle tip and drop, thereby increasing drop stability and achieving a higher stirrer speed (up to 1700 rpm). The method used 0.9 μl of carbon tetrachloride as extractant solvent, 40 min extraction time, stirring at 1300 rpm and no salt addition. The enrichment factor of this method ranged from 540 to 830. The linear ranges were 0.01–100 μg/l (four orders of magnitude) and limits of detection were 0.001–0.005 μg/l for most of analyte. The relative standard deviation (RSD%) for 2 μg/l of OPPs in water by using internal standard was in the range 1.1–8.6% ( n = 5). The recoveries of OPPs from farm water at spiking level of 1.0 μg/l were 91–104%.

Determination of chromium(III) in water by solid-phase microextraction with a polyimide-coated fiber and gas chromatography-flame photometric detection

A method for the determination of trace Cr(III) in aqueous solution by solid-phase microextraction (SPME) coupled with gas chromatography (GC)-flame photometric detection (FPD) was developed. Aqueous Cr(III) was first converted to the volatile chromium trifluoroacetylacetonate (Cr(tfa)3) by derivatization with 1,1,1-trifluoroacetylacetone (Htfa), followed by SPME extraction using a polyimide-coated silica fiber. The distribution constants (K) of derivatized cis- and trans-Cr(tfa)3 between the polyimide phase and aqueous phase were 2012 and 2214, respectively. The two Cr(tfa)3 isomers extracted can be efficiently separated by a DB-210 GC column within 9 min. Selective detection of Cr was performed by a FPD equipped with a 385-nm long-pass filter. Linearity (r> 0.99) over the concentration range 5-300 ng ml(-1) Cr was obtained and the limit of detection was 2 ng ml(-1) Cr. The relative standard deviation was 7% at 10 ng ml(-1) Cr (n = 5). Applicability of this method to water analysis was tested by analyzing the chromium content in a reference standard water sample and an industrial effluent.

Survey of butyltin compounds in 12 types of foods collected in China

Twelve representative food types including beans, fruit, vegetables, fish, meat, potatoes, sugar, beverages, alcohol, eggs, milk and corn were collected from four districts in China for the analysis of butyltin compounds. The hyphenated system of capillary gas chromatography-flame photometric detector using quartz surface-induced tin emission was used to measure propylated butyltins in various samples. Low levels (ng g−1) of butyltin compounds were found in some samples and possible sources of contamination and their significance are discussed.

Determination of Volatile Sulfur Compounds in Beverage and Coffee Samples by Purge-and-Trap On-Line Coupling with a Gas Chromatography-Flame Photometric Detector

A sensitive and fast analytical method using purge-and-trap on-line coupling with gas chromatography was developed for the determination of trace volatile sulfur compounds including dimethyl sulfide (DMS), ethyl-methyl sulfide (EMS), and dimethyl disulfide (DMDS) in beverage and coffee samples. The analytes were purged for 12 min from the sample by high purity nitrogen at a flow rate of 35 KPa and preconcentrated in the cooled fused-silica capillary trap at −75 °C. The NaCl content in the samples was maintained at 10%. The volatile sulfur compounds were separated with an Agilent-6890 gas chromatograph by a suitable temperature program and detected by means of a flame photometric detector (FPD). The detection limits were 80 ng L−1 for DMS, 80 ng L−1 for EMS, and 100 ng L−1 for DMDS, respectively. This method was successfully applied to the determination of volatile sulfur compounds in different beverage and coffee samples.

Sampling and Analysis of Butyltin Compounds in Air Using Gas Chromatography and Flame Photometric Detection

Organotin compounds are used in a variety of applications including stabilizers, catalysts, antifouling agents, and biocides. Because of the widespread use of organotin compounds in industry and their wide range of toxic effects, it is important to measure worker exposure to specific organotin compounds. Three butyltin compounds were selected for this study—butyltin trichloride, dibutyltin dichloride, and tri-butyltin chloride. These three compounds are typically present in the same work environment; therefore, developing a sampling and analytical method that would allow all three butyltin compounds to be sampled and analyzed simultaneously was desired. A derivatization procedure using sodium tetraethyl-borate (STEB) was selected for study and validation. The validation study demonstrated that sampling using the Occupational Safety and Health Administration (OSHA) Versatile Sampler (OVS) with XAD-2 resin sorbent and analysis using gas chromatography/flame photometric detection (GC/FPD) can be used to evaluate worker exposures to specific butyltin chlorides over the range of 5 to 270 μg/m3 collected at a flowrate of 0.25 L/min over a 3-hour period for a 45-L air sample. Breakthrough studies at 1.5 times the occupational exposure guideline (OEG) of 0.05 mg/m3 showed that samples could be collected at flowrates up to 0.5 L/min for 12 hours without breakthrough. The 14-day storage stability study showed apparent degradation of tributyltin and monobutyltin within a 3-day storage period at both ambient and refrigerated temperatures. There was no further degradation from 3 to 14 days. The stability of dibutyltin was unaffected by storage condition over the 14-day storage study. Subsequent stability studies incorporating a spiking solution control sample were conducted extending the stability study out to 27 days. These data show that all three butyltins were stable at either ambient or refrigerated conditions.

Sorption of tributyltin in seawater by municipal solid waste compost

AbstractThe use of municipal solid waste (MSW) compost as a sorbent for tributyltin (TBT) in seawater was investigated. TBT‐contaminated seawater, both artificially prepared and that collected from Msida Creek yacht marina (Malta), was allowed to percolate through untreated and water‐washed columns of compost and then analysed for organotins using gas chromatography‐flame photometric detection. About 90% of dissolved TBT ranging in concentration from about 800 to 8000 ngSnl−1 was sorbed by treating 500 ml solutions with 100 g untreated compost. On the other hand, no detectable breakthrough of TBT was observed from compost that had previously been washed by water to remove soluble organic matter. Breakthrough of TBT from unwashed compost is thought to be due to formation of complexes between the soluble organic matter in compost and aquated TBT, which renders the organotin more hydrophilic. The use of washed MSW compost as sorbent for the purification of TBT‐contaminated waters generated in large quantity during hull‐cleaning activities in drydocks is suggested as a mitigatory measure against the impact of TBT on the coastal marine environment. Copyright © 2001 John Wiley &amp; Sons, Ltd.

Glucosinolate content and isothiocyanate evolution--two measures of the biofumigation potential of plants.

A total of 570 lyophilised Brassica root and shoot tissue samples were hydrolyzed, and the liberated isothiocyanates (ITCs) were analyzed by gas chromatography-flame photometric detection (GC-FPD). Glucosinolates (GSLs) were extracted from samples of the same tissues and analyzed by high-performance liquid chromatography (HPLC). The concentrations of six GSLs/ITCs (2-propenyl, 3-butyl, 4-pentenyl, benzyl, 4-methylthiobutyl, and 2-phenylethyl) as determined by the two techniques were compared. In 79% of the samples, the concentration of GSLs in the tissues was greater than that of the ITCs released on hydrolysis. Several possible reasons for the difference are proposed, including the effect of tissue storage time, hydrolysis of GSLs may be less efficient than the GSL extraction procedure, or some of the ITCs formed reacted with plant proteins and amino acids in the sample and were therefore not detected in the extract. GSL concentration in plant tissues is used to estimate the biofumigation potential of the plant tissue, whereas the actual biofumigation effect is thought to be due to the ITCs formed by hydrolysis of the plant-based GSLs. The variation between ITC and GSL values therefore has implications for the assessment of the biofumigation potential of the plant tissue.