Analytical Method for Determination of Fipronil and its Metabolites in Vegetables Using the QuEChERS Method and Gas Chromatography/Mass Spectrometry

2015 ◽  
Vol 98 (2) ◽  
pp. 464-471 ◽  
Author(s):  
Ramandeep Kaur ◽  
Kousik Mandal ◽  
Rajinder Kumar ◽  
Balwinder Singh
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Ethyl Acetate ◽  
Analytical Method ◽  
Capillary Column ◽  
Gas Chromatography Mass Spectrometry ◽  
Quechers Method ◽  
Safe Method ◽  
Repeatability And Reproducibility

Abstract An easy, simple, and efficient analytical method was validated for the determination of residues of fipronil and its metabolites in different vegetables comprising brinjal, cabbage, capsicum, cauliflower, okra, and tomato. The Quick, Easy, Cheap, Rugged and Safe method was used for the extraction and cleanup of fipronil and its metabolites on these vegetables. Final clear extracts of ethyl acetate were concentrated under vacuum and reconstituted into acetone, and residues were determined by GC/MS with an Rtx-5 capillary column. The retention times of desulfinyl, sulfide, fipronil, sulfone, and amide were 11.8, 15.8, 16.4, 19.7, and 24.1 min, respectively. The average recoveries obtained for fipronil and its metabolites at different spiking levels were determined to be above 85% in all samples. The repeatability and reproducibility in different matrixes ranged from 1.36 to 5.42 and 1.75 to 4.53%, respectively, for fipronil and its metabolites. The LOQ of this method was 0.01 mg/kg and LOD was 0.003 mg/kg.

scholarly journals Development, Optimization and Validation of a Sustainable and Quantifiable Methodology for the Determination of 2,4,6-Trichloroanisole, 2,3,4,6-Tetrachloroanisole, 2,4,6-Tribromoanisole, Pentachloroanisole, 2-Methylisoborneole and Geosmin in Air

Processes ◽  
2021 ◽  
Vol 9 (9) ◽  
pp. 1571
Author(s):  
Patricia Jové ◽  
Marina Vives-Mestres ◽  
Raquel De Nadal ◽  
Maria Verdum
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
High Temperature ◽  
Thermal Desorption ◽  
Mass Spectrometric ◽  
Gas Chromatography Mass Spectrometry ◽  
Air Analysis ◽  
Good Linearity ◽  
Repeatability And Reproducibility

Compounds 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), 2,4,6-tribromoanisole (TBA) and pentachloroanisole (PCA), 2-methylisoborneol (2MIB) and geosmin (GSM) have been reported as being responsible for cork and wine taint. A sustainable method based on thermal desorption-gas chromatography–mass spectrometry (TD-GC/MS) has been developed and optimized, taking into account desorption parameters and chromatographic and mass spectrometric conditions. The combination of parameters that jointly maximized the compound detection was as follows: desorption temperature at 300 °C, desorption time at 30 min, cryo-temperature at 20 °C and trap high temperature at 305 °C. The proposed methodology showed a good linearity (R ≤ 0.994) within the tested range (from 0.1 to 2 ng) for all target compounds. The precision expressed as repeatability and reproducibility was RSD < 10% in both. The limits of quantification ranged from 0.05 to 0.1 ng. The developed methodology and the sampling rates (R-values) of all targeted compounds (from 0.013 to 0.071 m3 h−1) were applied to the air analysis of two wineries. The results showed that the developed methodology is a sustainable and useful tool for the determination of these compounds in air.

Determination of Phytosterols in Butter Samples by Using Capillary Column Gas Chromatography

1987 ◽  
Vol 70 (5) ◽  
pp. 912-915 ◽  
Author(s):  
Randall L Smith ◽  
Darryl M Sullivan ◽  
Earl F Richter
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Retention Time ◽  
Capillary Column ◽  
Limit Of Detection ◽  
Packed Column ◽  
Gas Chromatography Mass Spectrometry ◽  
Positive Bias ◽  
Capillary Column Gas Chromatography

Abstract A positive bias in the gas chromatographic (GC) analysis of butter for β-sitosterol was discovered when attempting to confirm values by gas chromatography/mass spectrometry (GC/MS). The source of the problem was traced to an interfering material that was not effectively separated by packed column GC. Because capillary columns are known to provide superior separation, they were substituted for packed columns in the assay, and instrument parameters were modified accordingly. A compound with a similar retention time, identified by GC/MS as lanosterol, was separated from β-sitosterol by the capillary column. The capillary column technique was applied to over 300 butter samples. The results indicate that the method can accurately quantitate β-sitosterol in butter with no known interferences. The limit of detection for this method is 1 mg/100 g. Recoveries at a level of 3 mg/100 g averaged 98% with a coefficient of variation of 3.45%

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