Gas chromatography‐mass spectrometry analysis of the herbicide clopyralid in differentially cultivated soils

Schütz, Stefan; Weißbecker, Bernhard; Hummel, H. E.

doi:10.1002/etc.5620150304

Cited by 4 publications

(4 citation statements)

References 11 publications

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“…The regulatory analytical methods for the determination of clopyralid from water samples, soil, and compost include gas chromatography (GC) [3][4][5][6][7][8][9][10] and liquid chromatography (LC). [11][12][13][14][15] Since clopyralid has a carboxylic group, the GC analysis required also the derivatization of the analyte as methyl ester, 4,6 1-butyl ester, 3,5,7 pentauorobenzyl ester 8 or silyl derivatives.…”

Section: Introductionmentioning

confidence: 99%

“…Usually, the extraction performs clean up and concentration in one step. The most applied extraction technique of clopyralid from water with organic solvents was carried out in the presence of sodium chloride, 4,5 sodium hydroxide 6,8,9 or tetrabutylammoniumhydroxide. 7 An aliquot was acidied and then was partitioned with an organic solvent.…”

Section: Introductionmentioning

confidence: 99%

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Droplets-based microextraction assisted SPME for GC-MS analysis of polar compounds such as clopyralid in water

et al. 2014

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For the first time, we assessed the performance of liquid phase microextraction (LPME) with droplets of organic solvent that assists solid phase microextraction (SPME) with chemically bonded polydimethylsiloxane (PDMS) fiber for analysis by gas chromatography-mass spectrometry of trace amounts of polar compounds in water. Clopyralid was used as a target analyte. LPME with droplets was performed with dichloromethane and was compared with dispersive liquid-liquid microextraction (DLLME) by addition of acetone or methanol as disperser solvent to dichloromethane. The main factors potentially affecting the microextraction were optimized. The optimal volume of dichloromethane was 17 mL per mL of aqueous samples. The relative enrichment factor for LPME in the presence of dichloromethane droplets was 200 and decreased by addition of disperser solvent. Consequently, DLLME cannot be applied with this SPME fiber. A characteristic of the method is that LPME and SPME can be conducted simultaneously or in two steps in the same vial. The limit of detection and the limit of quantification were 0.02 mg L À1 and 0.07 mg L À1 , respectively for 7 mm chemically bonded PDMS fiber and mass spectrometric detection was also carried out.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Droplets-based microextraction assisted SPME for GC-MS analysis of polar compounds such as clopyralid in water

et al. 2014

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“…So, the presence of picloram in fruits was investigated [7], though the main interest was the detection of the herbicides and their degradation products in soils, either directly [3,5,6] or after derivatization [4].…”

Section: Introductionmentioning

confidence: 99%

Electrochemical Reduction of Pyridinic Herbicides Picloram and Clopyralid on a Mercury Pool Electrode

et al. 2005

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This paper presents the identification by GC/MS of the products obtained after the total reduction of picloram and clopyralid on a mercury pool electrode. The products found in the strongly acidic media reduction of picloram are 4-amino-3,5,6-trichloro-2-pyridinecarboxaldehyde, 4-amino-3,5,6-trichloro-2-pyridinecarbinol and 4-amino-3,5-dichloro-2-pyridinecarboxylic acid; at pH 3 -4 the first compound is substituted by 4-amino-3,5-dichloro-2-pyridinecarboxaldehyde. For clopyralid 3,6-dichloro-2-pyridinecarbinol was detected. Under the light of such products the overall reduction processes are discussed showing the partial reductive cleavage of chlorine atoms in both cases.

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“…Previous studies have quantitatively analyzed clopyralid in soil using gas chromatography–mass spectrometry (Schütz et al. 1996; Ahmad et al.…”

Section: Introductionmentioning

confidence: 99%

Use of liquid chromatography–tandem mass spectrometry for quantitative analysis of clopyralid in compost and forage

et al. 2009

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In this study, we first developed a technique to quantify clopyralid using liquid chromatography–tandem mass spectrometry (LC/MS/MS) and tested its performance for compost and corn plant samples. Then, we measured the uptake of clopyralid by forage corn grown on two types of soil mixed with clopyralid‐contaminated compost, in order to investigate the potential of ingestion of compost clopyralid by animals through forage crops. Because of the high recovery ratios (80–82% for compost and 98% for corn), sufficient theoretical quantification limits (5.0 and 1.7 μg kg−1 fresh matter, respectively) and close agreement with the bioassay method (73 μg kg−1 for LC/MS/MS and 80 μg kg−1 for bioassay), the LC/MS/MS method was considered to be of potential value for determining clopyralid in compost and plant materials. Corn plants took up clopyralid from soil (compost), with the amount and rate of uptake varying with soil types and application of activated carbon to soil. There is a need for quantifying clopyralid uptake by a range of forage crops under a range of cultivation conditions (e.g. climate, soil, management) to estimate clopyralid fluxes through the manure–forage–animal–manure pathway.

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Gas chromatography‐mass spectrometry analysis of the herbicide clopyralid in differentially cultivated soils

Cited by 4 publications

References 11 publications

Droplets-based microextraction assisted SPME for GC-MS analysis of polar compounds such as clopyralid in water

Droplets-based microextraction assisted SPME for GC-MS analysis of polar compounds such as clopyralid in water

Electrochemical Reduction of Pyridinic Herbicides Picloram and Clopyralid on a Mercury Pool Electrode

Use of liquid chromatography–tandem mass spectrometry for quantitative analysis of clopyralid in compost and forage

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