Determination of residual fipronil in chicken egg and muscle by LC–MS/MS

•Fipronil residues in chicken egg and muscle were extracted with acetronitrile.•C18 SPE cartridge was better than common sorbents for purifying fipronil.•A novel and reliable LC–MS/MS method was established to assay fipronil residue.•The CCα for fipronil in chicken egg and muscle was 0.002μgkg−1. A...

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Veröffentlicht in:Journal of chromatography. B, Analytical technologies in the biomedical and life sciences Analytical technologies in the biomedical and life sciences, 2016-03, Vol.1014, p.31-36
Hauptverfasser: Zhang, Meiyu, Bian, Kui, Zhou, Tong, Song, Xuqin, Liu, Qingying, Meng, Chenying, He, Limin
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container_title Journal of chromatography. B, Analytical technologies in the biomedical and life sciences
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creator Zhang, Meiyu
Bian, Kui
Zhou, Tong
Song, Xuqin
Liu, Qingying
Meng, Chenying
He, Limin
description •Fipronil residues in chicken egg and muscle were extracted with acetronitrile.•C18 SPE cartridge was better than common sorbents for purifying fipronil.•A novel and reliable LC–MS/MS method was established to assay fipronil residue.•The CCα for fipronil in chicken egg and muscle was 0.002μgkg−1. A simple, sensitive and reliable method was developed and applied to the residue analysis of fipronil in chicken egg and muscle by liquid chromatography-tandem mass spectrometry (LC–MS/MS). Chicken egg and muscle samples were extracted with acetronitrile, then salting out by dehydration with anhydrous magnesium sulfate and sodium chloride. The extracts were purified by the C18 solid phase extraction cartridge prior to analysis by LC–MS/MS. The matrix-matched calibration curve showed a good linear within the concentration range from 0.01 to 2.00μgkg−1 (r2≥0.999). The average recoveries of fipronil at three spiked levels of 0.01, 0.1 and 1.0μgkg−1 ranged from 79.7% to 98.0%, and the relative standard deviations were less than 8.8%. The decision limit (CCα) and detection capability (CCβ) of fipronil in chicken egg and muscle matrices were all 0.002μgkg−1 and 0.01μgkg−1, respectively. The method has also been successfully applied to monitoring fipronil in the real samples.
doi_str_mv 10.1016/j.jchromb.2016.01.041
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A simple, sensitive and reliable method was developed and applied to the residue analysis of fipronil in chicken egg and muscle by liquid chromatography-tandem mass spectrometry (LC–MS/MS). Chicken egg and muscle samples were extracted with acetronitrile, then salting out by dehydration with anhydrous magnesium sulfate and sodium chloride. The extracts were purified by the C18 solid phase extraction cartridge prior to analysis by LC–MS/MS. The matrix-matched calibration curve showed a good linear within the concentration range from 0.01 to 2.00μgkg−1 (r2≥0.999). The average recoveries of fipronil at three spiked levels of 0.01, 0.1 and 1.0μgkg−1 ranged from 79.7% to 98.0%, and the relative standard deviations were less than 8.8%. The decision limit (CCα) and detection capability (CCβ) of fipronil in chicken egg and muscle matrices were all 0.002μgkg−1 and 0.01μgkg−1, respectively. 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B, Analytical technologies in the biomedical and life sciences</title><addtitle>J Chromatogr B Analyt Technol Biomed Life Sci</addtitle><description>•Fipronil residues in chicken egg and muscle were extracted with acetronitrile.•C18 SPE cartridge was better than common sorbents for purifying fipronil.•A novel and reliable LC–MS/MS method was established to assay fipronil residue.•The CCα for fipronil in chicken egg and muscle was 0.002μgkg−1. A simple, sensitive and reliable method was developed and applied to the residue analysis of fipronil in chicken egg and muscle by liquid chromatography-tandem mass spectrometry (LC–MS/MS). Chicken egg and muscle samples were extracted with acetronitrile, then salting out by dehydration with anhydrous magnesium sulfate and sodium chloride. The extracts were purified by the C18 solid phase extraction cartridge prior to analysis by LC–MS/MS. The matrix-matched calibration curve showed a good linear within the concentration range from 0.01 to 2.00μgkg−1 (r2≥0.999). The average recoveries of fipronil at three spiked levels of 0.01, 0.1 and 1.0μgkg−1 ranged from 79.7% to 98.0%, and the relative standard deviations were less than 8.8%. The decision limit (CCα) and detection capability (CCβ) of fipronil in chicken egg and muscle matrices were all 0.002μgkg−1 and 0.01μgkg−1, respectively. 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subjects Animals
Calibration
Cartridges
Chicken
Chickens
Chickens - metabolism
Chromatography
Chromatography, High Pressure Liquid - methods
Egg
Eggs - analysis
Fipronil
Insecticides - analysis
Limit of Detection
Liquid chromatography–tandem mass spectrometry
Liquids
Monitoring
Muscles
Muscles - chemistry
Pyrazoles - analysis
Residue
Solid Phase Extraction - methods
Standard deviation
Tandem Mass Spectrometry - methods
title Determination of residual fipronil in chicken egg and muscle by LC–MS/MS
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