Solid-phase microextraction for the determination of systemic and non-volatile pesticides in river water using gas chromatography with nitrogen–phosphorous and electron-capture detection

Sampedro, M. Carmen; Martín, Òscar Miró; Armentia, C. López de; Goicolea, M. Aránzazu; Rodríguez, Esther; Balugera, Zuriñe Gómez de; Costa-Moreira, J; Barrio, Ramón J.

doi:10.1016/s0021-9673(00)00746-9

Cited by 42 publications

(18 citation statements)

References 34 publications

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“…[16][17][18][19] From Tables 1 and 2, one can observe that compounds with higher octanol-water partition coefficient (log Kow) and low solubilities in water, such as chlorpyrifos, a-endosulfan and b-endosulfan, were the more extensively adsorbed when the PDMS fiber is used due to the higher affinity to the non-polar fiber coating. Compounds with higher polarities such as malathion and diazinon were adsorbed at a higher percentage (65 -80%) by PA in relation to PDMS fiber.…”

Section: Resultsmentioning

confidence: 99%

“…17 Another limitation of the PA fiber for the extraction of OCPs and OPPs is the more polar character of its coatings. Various authors [18][19][20] have shown that the diffusion coefficient of an analyte is higher in the 100 mm PDMS fiber than in the 85 mm PA fiber. As has been reported, for quantitative analysis it is not necessary for the analytes to reach equilibrium as long as the extractions are carefully timed and the mixing conditions and volumes remain constant.…”

Section: Effect Of Extraction Time and Temperaturementioning

confidence: 99%

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Optimization of Headspace Solid-Phase Microextraction for the Determination of Pesticide Residues in Vegetables and Fruits

2008

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Pesticides, including organochlorine pesticides (OCPs) and organophosphorous pesticides (OPPs) are examples of wellknown environmental contaminants. OPPs are used as a substitute for OCPs in many countries nowadays because they can degrade more easily in the environment. Although OPPs as a whole are not the most toxic pollutants, they can be traced to a wide range of surface water, fruits, vegetables and foodstuff. 1For fast monitoring of the environmental contamination caused by OCPs and OPPs and to accomplish risk assessment, more sensitive, rapid and simple analytical methods are paramount.Liquid-liquid extraction (LLE) and solid-phase extraction (SPE) are the most popular methods for extracting pesticides. However, they are time consuming and labor-intensive, and require large volumes of sample and solvents. In addition, because pesticides generally are present at ppt levels, mixed with other contaminants at higher concentrations, interfering compounds can produce extraneous peaks. LLE and SPE can carry contaminants into the final sample, producing a high background. 2-4Solid-phase microextraction (SPME), developed by Kataoka et al.,5 has received an increasing amount of attention at the analytical level in numerous scientific disciplines. 6 It is simple 6,7 and, as will be discussed later, offers great flexibility. In comparison with direct SPME, headspace (HP) SPME can shorten the time of extraction significantly because the diffusion rate of the analytes in gaseous phase is faster than that in the aqueous phase.1 Only a few references on the application of HS-SPME for the determination of OCPs and OPPs in fruit and vegetable samples can be found. 8,9 Most applications are based on the preparation of fruit or vegetable juices and analysis of target compounds by directly dipping of the SPME fibers into the slurry. [9][10][11][12][13][14] However several disadvantages related to fiber stability and sensitivity have been pointed out. Such problems can be overcome if headspace SPME is applied. Since the fiber is not in contact with the sample, background adsorption and matrix effects can be reduced, which also enhances the life expectancy of the SPME fibers. The objectives of this study are to evaluate the HS-SPME process by comparing two coating materials and to optimize the main parameters affecting the HS-SPME. Finally, we intended to develop an efficient multi-residue method on the basis of HS-SPME to extract each selected pesticide in fruit and vegetable samples. Experimental Chemicals and reagentsEight pesticides standards which are popular used by local farmers in vegetable and fruit cultivation 15 were > 95% pure and were purchased from AccuStandard Inc., USA. Stock solutions of each pesticide were prepared. Working standard solutions were prepared daily by volume dilution in distilled water. In the calibration and quantitation studies, an internal standard, 1-chloro-4-fluorobenzene, 200 mg/L which is effective as a surrogate to compensate the data of all 8 kinds of pesticides was added to each sample...

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Section: Resultsmentioning

confidence: 99%

Section: Effect Of Extraction Time and Temperaturementioning

confidence: 99%

Optimization of Headspace Solid-Phase Microextraction for the Determination of Pesticide Residues in Vegetables and Fruits

2008

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“…Gas Chromatography using GC-NPD (Sampledro et al, 2000;Beltran et al, 1998;Lopez et al, 1998;China Town Construction Guild Standard, 2001) coupled with SPE and saltout method determined concentrations of OPPs in surface water of Hangzhou as shown in Table II.…”

Section: Monitoring Of Organic Pesticidesmentioning

confidence: 99%

Risk Assessment of Organic Pesticides Pollution in Surface Water of Hangzhou

Sun

Zhu

Dong³

2006

Environ Monit Assess

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Advances in research on pollution of organic pesticides (OPs) in surface water, pollution survey and risk assessments of organochlorine pesticides (OCPs) and organophosphorus pesticides (OPPs) of surface water in Hangzhou are conducted. Total concentrations of dichloro-diphenyl-trichloroethane (DDT) and hexachloride-benzene (HCH) in surface water were observed to be 0-0.270 microg/L and 0-0.00625 microg/L respectively. DDE, as a metabolite of DDT and many species of OPP(S) were determined in some samples of surface water. Parathion, the main pollutant among OPPs in surface water of Hangzhou, was observed to be 0-0.445 microg/L. Based on these experimental results, health risk assessments on the organic pollution are developed. It is observed that the total risk "R (T)" at present time of surface water in Hangzhou is mainly contributed by organophosphorus pesticides, especially Parathion; HCH and DDT are not the main contaminants; on the contrary, organophosphorous pesticides, especially Parathion, must be of concern at the present time.

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“…In the literature liquid-liquid extraction (LLE) [18], solidphase extraction (SPE) [19] and solid-phase microextraction (SPME) [20] are described as sample preparation for endosulfan determination. Although LLE gives sometimes better recovery results [21], there is a general tendency to use SPE as an extraction method because this method avoids the use of high amounts of toxic organic solvents.…”

Section: A B Deger · T J Gremm · F H Frimmel · L Mendezmentioning

confidence: 99%

Optimization and application of SPME for the gas chromatographic determination of endosulfan and its major metabolites in the ng L−1 range in aqueous solutions

et al. 2003

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In the present study an analytical method was optimized for the determination of alpha-endosulfan, beta-endosulfan, endosulfan sulfate, endosulfan ether and endosulfan lactone in small volumes of environmental aqueous samples using solid-phase microextraction (SPME) and gas chromatography-electron capture detection (GC-ECD). A 100 micro m polydimethylsiloxane (PDMS) phase was used for the extraction. The limit of detection (LOD) for the analytes varied between 0.01 and 0.03 micro g L(-1) with a relative standard deviation of 3 to 11%. The influence of the ionic strength on the extraction efficiency was investigated for the individual compounds. alpha-Endosulfan, beta-endosulfan, endosulfan sulfate and endosulfan ether were extracted successfully without salt addition. The extraction efficiency of endosulfan lactone was improved with 30% NaCl content. A general decrease in extraction efficiency for alpha-endosulfan, beta-endosulfan, endosulfan sulfate and endosulfan ether with high NaCl content (20-30%) in the solution was observed due to glass surface adsorption. No effect of dissolved organic material (DOM) on the extraction efficiency was observed. The extraction coefficients changed between Log K=2.17 and 3.33. A sample from the Antarctic region was analyzed using the optimized GC-ECD/SPME method. To confirm the results obtained for the real sample a GC with a mass spectrometer (MS) was used. Endosulfan sulfate, the most toxic metabolite of endosulfan, was found in the sample at a concentration of 0.3 micro g L(-1).

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Solid-phase microextraction for the determination of systemic and non-volatile pesticides in river water using gas chromatography with nitrogen–phosphorous and electron-capture detection

Cited by 42 publications

References 34 publications

Optimization of Headspace Solid-Phase Microextraction for the Determination of Pesticide Residues in Vegetables and Fruits

Optimization of Headspace Solid-Phase Microextraction for the Determination of Pesticide Residues in Vegetables and Fruits

Risk Assessment of Organic Pesticides Pollution in Surface Water of Hangzhou

Optimization and application of SPME for the gas chromatographic determination of endosulfan and its major metabolites in the ng L−1 range in aqueous solutions

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