2009Physical Testing and Chemical AnalysisRequires access

GC-MS Determination of Residual Endosulfan and Chlorpyrifos in Aquatic Products

LI Zuo-qing

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Abstract

Residual amounts of endosulfan and chlorpyrifos in aquatic products(taking eel as testing sample) were determined by GC-MS with negative chemical ionization(NCl) source.The smashed and slurried sample was extracted with ethyl acetate,and the extract obtained was evaporated to dryness at 40 ℃.The residue was taken up with acetonitrile and purified by passing through the acidic aluminum oxide chromatographic column,and the acetonitrile solution was dried at 50 ℃ by N2-blowing.The dried residue was dissolved in a definite volume of n-hexane and used for GC-MS determination with SIM mode.Ranges of linearity of standard curves for the 3 compounds(i.e.,chlorpyrifos,α-endosulfan and β-endosulfan) found were all in the range of 0.2 μg·kg-1 to 10.0 μg·kg-1.Detection limit(3S/N) of the method was found to be 0.5 μg·kg-1.Values of recovery found were in the range of 81%-95%,and values of RSD′s(n=8) were less than 5%.

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Residual amounts of endosulfan and chlorpyrifos in aquatic products(taking eel as testing sample) were determined by GC-MS with negative chemical ionization(NCl) source.The smashed and slurried sample was extracted with ethyl acetate,and the extract obtained was evaporated to dryness at 40 ℃.The residue was taken up with acetonitrile and purified by passing through the acidic aluminum oxide chromatographic column,and the acetonitrile solution was dried at 50 ℃ by N2-blowing.The dried residue was dissolved in a definite volume of n-hexane and used for GC-MS determination with SIM mode.Ranges of linearity of standard curves for the 3 compounds(i.e.,chlorpyrifos,α-endosulfan and β-endosulfan) found were all in the range of 0.2 μg·kg-1 to 10.0 μg·kg-1.Detection limit(3S/N) of the method was found to be 0.5 μg·kg-1.Values of recovery found were in the range of 81%-95%,and values of RSD′s(n=8) were less than 5%.

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Available abstract

Residual amounts of endosulfan and chlorpyrifos in aquatic products(taking eel as testing sample) were determined by GC-MS with negative chemical ionization(NCl) source.The smashed and slurried sample was extracted with ethyl acetate,and the extract obtained was evaporated to dryness at 40 ℃.The residue was taken up with acetonitrile and purified by passing through the acidic aluminum oxide chromatographic column,and the acetonitrile solution was dried at 50 ℃ by N2-blowing.The dried residue was dissolved in a definite volume of n-hexane and used for GC-MS determination with SIM mode.Ranges of linearity of standard curves for the 3 compounds(i.e.,chlorpyrifos,α-endosulfan and β-endosulfan) found were all in the range of 0.2 μg·kg-1 to 10.0 μg·kg-1.Detection limit(3S/N) of the method was found to be 0.5 μg·kg-1.Values of recovery found were in the range of 81%-95%,and values of RSD′s(n=8) were less than 5%.

Key concepts: Chemistry, Chromatography, Endosulfan, Chlorpyrifos, Residue (chemistry), Acetonitrile, Detection limit, Ethyl acetate

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