Analysis of bioaccessible concentration of trace elements in plant based edible materials by INAA and ICPMS methods

The total metal concentration and bioaccessible concentration of Cr, Mn, Fe, Cu, Zn, Se in Momordica charantia, Asparagus racemosus, Terminalia arjuna and Syzyzium cumini were measured by instrumental neutron activation analysis and by inductively coupled plasma mass spectrometry analysis (ICP-MS). The bioaccessible concentrations were determined in the gastrointestinal digest obtained after treating dried powdered samples sequentially in gastric and intestinal fluid of porcine origin at physiological conditions. The bioaccessible concentration of Fe was in the range of 58–67 mg kg^?1, Mn was 10.2–14.6 mg kg^?1, Cu was 3.7–4.8 mg kg^?1 and Zn was 10.6–18.4 mg kg^?1, were within the safety limits set for vegetable food stuff set by Joint FAO/WHO. The bioaccessibility of Zn, an essential element, was high (40–50 %) in M. charantia and in S. cumini. In addition, the total metal contents and bioaccessible concentration of Ni, Se, Cd and Pb in these samples were measured by ICP-MS. The total Cd content in S. cumini (2.6 ± 0.2 mg kg^?1) and its bioaccessible concentration (0.6 mg kg^?1) were strikingly high as compared to the other samples. Though total Hg contents were determined by ICP-MS, but their bioaccessible concentrations were below the detection limit (0.036 mg kg^?1).     

Applications of EDXRF and INAA techniques for studying impact of industries to the environment

In this study we present quantitative elemental analysis techniques like energy dispersive X-ray fluorescence analysis and instrumental neutron activation analysis to assess the impact of industrial discharge on environment. Two cases are discussed, i.e., (a) enrichment of zinc levels in the soil (1080 ± 76 mg kg^?1) and zinc uptake ranging between 628 and 40 mg kg^?1 in edible plants and cereals grown in agricultural fields near an active zinc smelter, Rajasthan; (b) depth-wise distribution of Cr, Pb and other metals in the sediment core samples from Sundarban wetland, West Bengal, indicating waste discharge from tanneries and other industries.     

Transfer of Metals from Soil to Crops in an Area near a Coal Gangue Pile in the Guqiao Coal Mine,China

A field survey was conducted to investigate the metal contamination in coal gangue, soils, and crops (rice and soybeans), and to evaluate the possible health risks to the local population through food chain transfer near a coal gangue pile in the Guqiao Coal Mine, China. Contamination levels of zinc, lead, cadmium, and copper in coal gangue, soils, and crops were measured, and bio-accumulation factors from soil to crops were determined; the health risks were calculated accordingly. Results showed that both coal gangue and soil contained high levels of cadmium (0.15 mg kg^?1and 0.20 mg kg^?1) exceeding the background value of the soil. The lead soil concentration was low (9.99 mg kg^?1), but lead in rice (0.38 mg kg^?1) exceeded the maximal permissible limit of 0.2 mg kg^?1. For some tissues of crops studied, there was a significant correlation between the bio-accumulation factor values and the corresponding soil metal concentrations that were best described by a power equation. Oral intake of zinc, cadmium, and copper through crops posed no health risk to local residents, although hazard indices for rice (0.87–2.88) and soybeans (0.06–0.09) suggested that ingestion of rice grains was unsafe for human health. Therefore, rice was inappropriate to be planted in the soil surrounding this coal mine.     

Analysis of triallate residue and degradation rate in wheat and soil by liquid chromatography coupled to tandem mass spectroscopy detection with multi-walled carbon nanotubes

A modified quick, easy, cheap, effective, rugged and safe (QuEChERS) method for the analysis of triallate residue in wheat and soil was developed and validated. Multi-walled carbon nanotubes were used as clean-up sorbent. The residual levels and dissipation rates of triallate in wheat and soil were determined by liquid chromatography–tandem mass spectrometry. The limit of quantification was established as 0.01, 0.02 and 0.05 mg kg^?1 for soil, wheat and wheat plant samples, respectively. The average recoveries of triallate ranged from 77% to 108% at fortified levels of 0.01–0.5 mg kg^?1 with relative standard deviations of 3.0–8.4% (n = 5). From residue trials at three geographical experimental plots in China, the results showed that the half-lives of triallate in soils were 1.13–1.63 days. For trials applied according to the label recommendation, the final residues of triallate in wheat at harvest time were all below 0.05 mg kg^?1 (the maximum residue levels of China, Japan, Korea and the US).     

Determination of concentrations of chromium and other elements in soil and plant samples from leather tanning area by Instrumental Neutron Activation Analysis

Chromium, one of the toxic elements, along with other elements has been determined in samples of soil and plant (leaves and seeds) from Jajmau Area, Kanpur district, India, which is irrigated with effluent waste water from leather tanning industries. Soil and plant samples were collected from these areas and analyzed by Instrumental Neutron Activation Analysis (INAA) using high flux reactor neutrons and high resolution gamma-ray spectrometry. Concentrations of fifteen elements in soil and five elements in plant samples were determined by relative method. Chromium concentrations were found to be in range of 45–3,900 mg kg^?1in soil samples and 14–83 mg kg^?1 in plant samples. This study showed that Cr is present in significant amounts, in the soil as well as in the plant samples, near to the leather tanning area. As a part of quality control work, IAEA reference material (RM) SL-3 and NIST standard reference material (SRM) 1645 were analyzed and the quality of the results has been evaluated by calculating % deviations from recommended/literature/certified values.     

QuEChERS and solid phase extraction methods for the determination of energy crop pesticides in soil,plant and runoff water matrices

QuEChERS and solid phase extraction (SPE) methods were applied for determining four herbicides (metazachlor, oxyfluorfen, quizalofop-p-ethyl, quinmerac) and one insecticide (α(±)-cypermethrin) in runoff water, soil, sunflower and oilseed rape plant matrices. Determination was performed using gas chromatography mass spectrometry (GC-MS), whereas high-pressure liquid chromatography mass spectrometry (HPLC-MS) was used for quinmerac. In all substrates linearity was evaluated using matrix-matched calibration samples at five concentration levels (50–1000 ng L^?1 for water, 5–500 μg kg^?1 for soil and 2.5–500 μg kg^?1 for sunflower or oilseed rape plant). Correlation coefficient was higher than 0.992 for all pesticides in all substrates. Acceptable mean recovery values were obtained for all pesticides in water (65.4–108.8%), soil (70.0–110.0%) and plant (66.1–118.6%), with intra- and inter-day RSD% below 20%. LODs were in the range of 0.250–26.6 ng L^?1 for water, 0.10–1.8 μg kg^?1 for soil and 0.15–2.0 μg kg^?1 for plants. The methods can be efficiently applied for field dissipation studies of the pesticides in energy crop cultivations.     

Persistence of trifloxystrobin and tebuconazole in banana tissues and soil under the semi-arid climatic conditions of Karnataka,India

Trifloxystrobin and tebuconazole are used for control of Sigatoka leaf spot disease of banana. This study was conducted to evaluate residue persistence of the fungicides in/on banana fruit, other edible parts and soil after spray application of the combination formulation, Nativo 75 WG, at the standard dose, 87.5 + 175 and double dose, 175 + 350 g a.i. ha^?1. The fungicides were extracted from banana and soil with acetone, partitioned into dichloromethane and cleaned-up using activated charcoal for trifloxystrobin and primary/secondary amine (PSA) for tebuconazole samples. The limit of quantification of the method was 0.05 mg kg^?1 for both fungicides. Initial residues of trifloxystrobin were 0.444 and 0.552 mg kg^?1 in/on banana with peel (whole fruit), which reached <0.05 and 0.065 mg kg^?1 after 30 days from treatment at the standard and double doses, respectively. Tebuconazole residues were 0.636 and 960 mg kg^?1 initially and reduced to 0.066 and 0.101 mg kg^?1 after 30 days. Trifloxystrobin and tebuconazole degraded with the half-life of about 11 days. Trifloxystrobin or its metabolite was not detected in the fruit pulp. Tebuconazole being systemic in nature moved to the fruit pulp which was highest on the 3rd day (0.103 and 0.147 mg kg^?1) and remained for 15 days. Matured banana fruit, flower, pseudostem and field soil were free from fungicide residues. For consumption of raw banana 43 days pre-harvest interval (PHI) is required after treatment of the combination formulation. Therefore application of the fungicides towards maturity stage of the fruits may be avoided.     

Persistence and dissipation of fluopicolide and propamocarb on cabbage and soil under semi-arid climatic conditions

Persistence and dissipation of fluopicolide and propamocarb were studied on cabbage and soil as per good agricultural practices over a period of 2 years. A modified QuEChERS analytical method in conjunction with gas chromatography (GC) and GC–mass spectrometry was used for analysis of fluopicolide and its metabolite, 2,6-dichlorobenzamide, and propamocarb in cabbage and soil. The results of the method validation were satisfactory with recoveries within 74.5–100.81% and relative standard deviations 4.8–13.9% (n = 6). The limit of detection (LOD) and limit of quantification (LOQ) of both fluopicolide and 2,6-dichlorobenzamide were 0.003 µg mL^?1 and 0.01 mg kg^?1, respectively. The LOD and LOQ of propamocarb were 0.03 µg mL^?1 and 0.1 mg kg^?1, respectively. During 2013, the initial residue deposits of fluopicolide on cabbage were 0.60 and 1.48 mg kg^?1 from treatments at the standard and double doses of 100 and 200 g a.i. ha^?1 which dissipated with the half-life of 3.4 and 3.7 days. During 2014, the residues were 0.49 and 1.13 mg kg^?1 which dissipated with the half-life of 4.2 and 5.1 days. Propamocarb residues on cabbage were 5.36 and 12.58 mg kg^?1 in the first study (2013) and 4.85 and 10.26 mg kg^?1 in the second study (2014) from treatments at the standard and double doses of 1000 and 2000 g a.i. ha^?1, respectively. The residues dissipated with the half-life of 4–5.5 days. The preharvest interval, the time required for fluopicolide + propamocarb residues to dissipate below the maximum residue limits (notified by EU) at the standard dose, was 11.8 and 14 days during 2013 and 2014. Residue of 2,6-dichlorobenzamide was always <LOQ in cabbage. Residues of fluopicolide, 2,6-dichlorobenzamide and propamocarb were <LOQ in field soil at harvest.     

Dissipation rates of saisentong residues in fresh tobacco,tobacco powder and soil determined by high-performance liquid chromatography coupled with diode array detection

Two independent field trials were performed in Guizhou and Hunan, China in 2013 to investigate the dissipation and residue levels of saisentong in tobacco and soil. A novel and accurate method using high-performance liquid chromatography with diode array detection was developed and validated to determine saisentong levels in tobacco and soil. The average recovery of saisentong at fortification levels of 0.5, 2.5, 5.0 and 50.0 mg kg^?1 in fresh tobacco ranged from 75.92 to 107.40% with a relative standard deviation (RSD) of 0.94 to 7.55%, that at fortification levels of 0.5, 2.0 and 5.0 mg kg^?1 in tobacco powder ranged from 74.96 to 94.43% with a relative standard deviation (RSD) of 4.38 to 8.14%, and that at fortification levels of 0.1, 0.5 and 5.0 mg kg^?1 in soil ranged from 86.90 to 100.0% with an RSD of 1.38 to 4.62%. The limit of detection (LOD) of saisentong was 0.15 mg?kg^?1 in tobacco and 0.03 mg kg^?1 in soil, and the limit of quantification (LOQ) was 0.5 mg kg^?1 in tobacco and 0.1 mg kg^?1 in soil, respectively. For field experiments, the half-lives of saisentong in tobacco from Guizhou and Hunan were 5.9 and 1.6 days, respectively; those in soil were 14.7 and 12.0 days, respectively. The results suggest that the saisentong dissipation curves followed the first-order kinetic. The terminal residues of saisengtong in tobacco ranged from 0.5 to 9.39 mg kg^?1 at pre-harvest intervals (PHI) of 7, 14 and 21 days.     

Dissipation and residue fate of kresoxim-methyl in tobacco leaves and soil under field conditions

The fate of kresoxim-methyl was studied in a tobacco field ecosystem, and a simple and reliable method was developed for the determination of kresoxim-methyl in soil, green and cured tobacco leaves. Kresoxim-methyl residues were extracted from samples with petroleum ether, and determined by gas chromatography (GC) coupled with an electron capture detector (ECD). Kresoxim-methyl (30% suspension concentration) was applied at 150 g a.i. ha^–1 (the recommended high dosage) and 225 g a.i. ha^–1 (1.5 times the recommended high dosage) in the experimental fields in Huishui and Changsha in China. The limits of detection (LODs) and limits of quantification (LOQs) of kresoxim-methyl in green tobacco leaves, cured tobacco leaves and soil were 0.012 and 0.04 mg kg^–1, 0.12 and 0.4 mg kg^–1, and 0.0015 and 0.005 mg kg^–1, respectively. The average recoveries were 84.5% to 95.7%, 79.8% to 94.3% and 83.3% to 93.8% with relative standard deviations (RSDs) less than 10% in green tobacco leaves at four spiked levels (0.04, 0.2, 2 and 8 mg kg^–1), cured tobacco leaves at three spiked levels (0.4, 1 and 10 mg kg^–1) and soil at three spiked levels (0.005, 0.05 and 0.5 mg kg^–1), respectively. The results showed that the half-lives of kresoxim-methyl in green tobacco leaves and soil were 1.2–5.3 days and 6.7–10.4 days, respectively. At harvest, kresoxim-methyl residues in cured tobacco leaves samples collected 21 days after the last application at the recommended dosage were below 1.0 mg kg^–1. These results could help establish appropriate application frequency and harvest intervals in the use of kresoxim-methyl on tobacco plants.     

DNA Damage and Effects on Antioxidative Enzymes in Earthworm (Eisenia fetida) Induced by Flumorph

Flumorph is an Oomycete fungicide, which is used extensively as an effective fungicide in vegetables and fruits, but little is known about its effect on nontarget soil organisms. In the present study, biochemical responses including changes in the activity of antioxidative enzymes catalase (CAT), superoxide dismutase (SOD), glutathione-S-transferase (GST), malondialdehyde (MDA), and DNA damage induced by flumorph were investigated in earthworms (Eisenis fetida). The CAT concentrations were stimulated at 5.0 mg kg^?1 over 28 days and inhibited at 10 and 20 mg kg^?1, except 10 mg kg^?1 on days 21 and 28 compared with the controls. The overall SOD activities were inhibited except 5 mg kg^?1 on day 28 and 10 mg kg^?1 on days 7 and 14. Meanwhile, the GST activities were stimulated on day 7 and decreased on the other days in summary. The MDA activities were increased notably at 5, 10, and 20 mg kg^?1 after 14 days. Clear dose-dependent DNA damage to Eisenia fetida was observed by olive tail moments in comet assay compared with controls. The results demonstrate that flumorph induces oxidative stress and DNA damage to earthworms, and the effects may be the important mechanisms of its toxicity.     

Determination of trace concentrations of thorium in uranium oxide matrix by epithermal instrumental neutron activation analysis

An epithermal instrumental neutron activation analysis (EINAA) method using cadmium filter was standardized to determine trace concentrations of thorium in four samples of uranium oxide (U₃O₈) samples. Samples and thorium standards, wrapped with cadmium foil, were irradiated at a reactor neutron flux of about 10¹² cm^?2 s^?1. Radioactive assay was carried out using a Compton suppressed anticoincidence gamma ray spectrometer consisting of HPGe-BGO detectors coupled to MCA. Concentrations of thorium in these samples were found to be in the range of 15–72 mg kg^?1. EINAA results were validated by determining thorium concentrations in uranium matrix by standard addition method. EINAA results were compared with those obtained by two wet chemical methods namely ion chromatography (IC) and inductively coupled plasma atomic emission spectrometry (ICP-AES). The results obtained by the three methods were found to be in good agreement, indicating further validity of the proposed EINAA method.     

Biodegradation of imidacloprid in sandy loam soil by Bacillus aerophilus

A study of the biodegradation of imidacloprid in soil was carried out under laboratory conditions. Sandy soil samples were fortified with imidacloprid at 50, 100 and 150 mg kg^?1 along with 45 x 10⁷ colony forming units (cfus) of Bacillus aerophilus and the samples were compared with unamended soil. The samples were extracted with acetonitrile, cleaned up by treatment with primary secondary amine sorbent and graphitised carbon black. The residues of imidacloprid and its metabolites were analysed by high performance liquid chromatography. The parent compound, imidacloprid, was found to be more persistent in both the treatments. Among metabolites, the highest values were obtained for urea and olefin while 5-hydroxy, 6-chloronicotinic acid (6-CNA), nitrosimine and nitroguanidine (NTG) were also observed in all the treatments in amended soil. In case of unamended (control) soil, 6-CNA was found to be the most persistent metabolite followed by olefin, urea, 5-hydroxy, nitrosimine and NTG metabolites. Total imidacloprid residues for control soil samples followed first-order kinetics at 50 and 150 mg kg^?1 but in case of control imidacloprid fortified at 100 mg kg^?1, the total residues of imidacloprid and its metabolites followed pseudo-first-order kinetics. The respective half-life value for 50 mg kg^?1 was 25.08 days and 30.10 days for both 100 and 150 mg kg^?1. However, total imidacloprid residues followed pseudo-first-order kinetics for its applications at 50, 100 and 150 mg kg^?1 in sandy loam soil amended with B. aerophilus. The half-life values for 50, 100 and 150 mg kg^?1 were worked out to be 14.33, 15.05 and 18.81 days, respectively. With the use of B. aerophilus, the reduction percentage of initial applied dose imidacloprid in sandy loam soil was found to be higher in all the three doses as compared to that of the control samples.     

International comparison of the determination of the mass fraction of cadmium, chromium, mercury and lead in polypropylene: the Comité Consultatif pour la Quantité de Matière pilot study CCQM-P106

The CCQM-P106 pilot study was organized by the inorganic working group of the Comité Consultatif pour la Quantité de Matière (CCQM) as a feasibility comparison to study the applicability of different analysis methods to the polypropylene sample and test the abilities of the participants for measuring the Cd, Cr, Hg and Pb in polypropylene. National Institute of Metrology P.R. China (NIM) acted as the coordinating laboratory of this pilot study. There were 21 laboratories that submitted the final results. The median values of the mass fraction of Cd, Cr, Hg and Pb were 36.12 mg kg^?1 (the median absolute deviation about the median (MADe) = 0.46 mg kg^?1), 252.5 mg kg^?1 (MADe = 3.4 mg kg^?1), 387.0 mg kg^?1 (MADe = 10.1 mg kg^?1) and 466.2 mg kg^?1 (MADe = 8.9 mg kg^?1), respectively. Isotope dilution mass spectrometry (IDMS), inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-optical emission spectrometry (ICP-OES), atomic absorption spectrometry (AAS), instrumental neutron activation analysis (INAA) and X-ray fluorescence (XRF) measurement methods were used, and microwave digestion was used by the most of the participants. In general, very good agreement of the results was observed. Moreover, compared to the results of other methods, the results of IDMS still showed less spread amongst laboratories and had a smaller uncertainty. In addition, the results of some analytes used by XRF and INAA also got satisfactory agreement with the median value.     

Phosphate effect on the content of selected elements in a lettuce variety grown at a contaminated soil

The purpose of this study was to evaluate the efficiency of superphosphate fertilizer in remediating a contaminated soil with potentially toxic elements. For this, different phosphorus doses were used in a number of lettuce plants. The element concentrations determined in their leaves were compared with those found in control lettuce plants. Instrumental neutron activation analysis was the analytical technique used to determine element concentration in lettuce leave samples. The application of 250 mg kg^?1 of P was the most effective treatment to reduce the concentrations of Br, Ca, Cd, Cl, Co, Cr, Fe, K, Mg, Mn, Sb and Zn in lettuce leaves.     

Residues and dissipation of guadipyr in rice ecological system

A modified QuEChERs method with liquid chromatography-tandem mass spectrometry for analysis of guadipyr residue and dissipation in rice matrices, paddy soil and paddy water was developed and validated. Mean recoveries and relative standard deviations in paddy soil, paddy water, rice plant, rice straw, rice hull and husked rice matrices at three spiking levels were 83.1–116.5% and 1.6–9.5%, respectively. The half-life of guadipyr was determined in 2 years at three different field sites in China via a dissipation experiment. The half-lives of guadipyr in paddy water were 0.22–0.37 days, 0.24–3.33 days in paddy soil and 0.44–1.90 days in rice plant. The terminal residues of guadipyr ranged from ND (concentrations of guadipyr were below limit of detection) to 50 μg kg^?1 in paddy soil, 10–470 μg kg^?1 in rice hull, ND70 μg kg^?1 in husked rice and ND to 110 μg kg^?1 in rice straw. The results would be helpful in fixing maximum residue limit of guadipyr, a new insecticide, in rice.     

Selenium content of Argentinean infant formulae and baby foods by pseudo-cyclic instrumental neutron activation analysis coupled to Compton suppression

The selenium levels of Argentinean infant formulae and baby food were measured using the 162-keV gamma-ray of ^77mSe (t _½ = 17.4 s) by a pseudo-cyclic instrumental neutron activation analysis (PC-INAA) method in conjunction with Compton suppression spectrometry (CSS). For comparison purposes, 5 selected infant formulae were also analyzed for selenium by a radiochemical neutron activation analysis (RNAA) method. The selenium levels for three samples agreed between ±2.8 and 6.5 % while the other two differed by 12 and 17 % which could perhaps be attributed to sample inhomogeneity. The selenium content of cow milk-based infant formulae varied from 42–146 μg kg^?1 compared to 52–63 μg kg^?1 for soy-based milk formulae. In the case of baby foods, the selenium levels varied from 34 to 74 μg kg^?1. The detection limits for selenium by PC-INAA–CSS for all the samples analyzed in this work were between 8.5 and 65 μg kg^?1 depending on the major elements present in the samples, while it was 20 μg kg^?1 for the RNAA method. The expanded uncertainty (κ = 2) of the PC-INAA–CSS method was 7.0 % at the end of cycle #4 for a sample containing 73.7 μg kg^?1 selenium compared to the RNAA value of 24.2 % for a sample of 67.0 μg kg^?1 selenium content.     

Residue dynamics of chlorpyrifos and cypermethrin in/on pomegranate (Punica granatum L.) fruits and soil

Study on the residue dynamics of chlorpyrifos and cypermethrin in/on pomegranate (Punica granatum L.) and soil was carried out by conducting supervised field trials as per good agricultural practices. A modified QuEChERS was used to extract the insecticides in pomegranate peel and aril and soil. The limit of quantification (LOQ) of chlorpyrifos and cypermethrin were 0.01 and 0.05 mg kg^?1, respectively. Residues of the insecticides remained on the fruit surface and movement to the edible part (aril) was not observed. The residues after treatment on fruit peel were 2.46 and 3.51 mg kg^?1 and 2.84 and 4.54 mg kg^?1 for chlorpyrifos and cypermethrin, respectively, from recommended and double dose treatments. Chlorpyrifos residues degraded faster compared to cypermethrin. The pre-harvest intervals (PHIs) of chlorpyrifos were 22 and 35 days and those of cypermethrin 50 and 73 days, respectively, at recommended and double dose treatments. In the experimental field soil after the second application chlorpyrifos residues were 0.21 and 0.46 mg kg^?1 and cypermethrin residues 0.15 and 0.36 mg kg^?1. At harvest, both pesticides showed residues below the LOQ. Based on this study, application of cypermethrin towards harvest may be avoided whereas chlorpyrifos can be applied with 22 days PHI.     

Concentration of arsenic in soil samples collected around the monazite processing facility, Thailand

Arsenic (As) in soil is a contaminant originated from human activities including pesticide use, mining and ore processing operations. In this work, As concentration in soil samples collected around the monazite processing facility, Pathum Thani, Thailand, was investigated. The collections of 24 soil samples were collected from the monazite processing area and 7 soil samples were collected from the control area without the processing activity of the same facility. Soils were digested with the mixture of HNO₃, HClO₄ and HF using a microwave digester. Inductively coupled plasma mass spectrometer (ICP-MS) equipped with an octopole reaction system (ORS) was used to determine the concentration of As in soils after the acid digestion. JB-3 (igneous rock) was the standard reference material used to check the accuracy of the method. It was found that the analytical results showed good agreement with the certified values. As concentration in soils collected from the monazite processing area ranged from 3.85 to 36.01 mg kg^?1 with the mean of 13.06 mg kg^?1. The concentration of As higher than the US EPA cancer soil screening level (22 mg kg^?1) was observed for only one sample. The control area showed As concentration varied from 9.59 to 14.19 mg kg^?1 with the mean of 11.97 mg kg^?1. The obtained results from this work were compared with the contaminated soil data of Amphoe Ron Phibun, Nakhon Si Thammarat, Thailand.     

Derivatization and Determination of MCPA in Soil by GC

A reliable and sensitive method for determination of MCPA in soil by derivatization through p-toluenesulfonic acid and 1,3-dichloro-2-propanol followed by gas chromatographic detection under ECD mode has been established. After treatment with hydrochloric acid, the soil samples were directly extracted without any clean-up with dichloromethane by vortexing. After derivatization and liquid–liquid extraction, the product was subjected to GC analysis. Under optimized conditions, recovery of MCPA reached 87–91%; intra- and inter-day precision values were recorded in the range 3.4–6.4% and 7.4–8.7%, respectively. Excellent linear relationship was observed within 0.1–10 μg mL^?1 (0.005–0.5 mg kg^?1) with linear correlation coefficient (R) of 0.9997. The LOD and LOQ were 0.001 and 0.0026 mg kg^?1, respectively, and the overall sensitivity for detection was found to be in the same range as with the conventional GC-MS technique.