2014Shipin anquan zhiliang jiance xuebaoRequires access

Determination of 11 hormones residues in chicken using QuEChERS sample preparation method with ultra performance liquid chromatography-tandem mass spectrometry

Lian Ying

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Abstract

Objective A multi-residue testing method was developed for the simultaneous determination of 4 androgens, 3 progesterones and 4 glucocorticoids in chicken using QuEChERS sample preparation method with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The homogenized sample extracted with ethyl acetate. The separation was performed on a phenomenex kinetex column by gradient elution after puring from dispersive-solid-phase extraction(d-SPE). The analysis of 11 analytes were operated by electrospray ionization mass spectrometry under the positive or negative mode using multiple reaction monitoring(MRM). Acetonitrile and water(containing 0.1% formic acid) were used as the mobile phase both in positive and negative. Results The correlation coeficients of calibration curves were over 0.991 in the corresponding concentration range. The average recoveries of the 11 analytes at three spiked concentration levels varied from 84.4% to 94.1% and the relative standard deviations(RSDs) varied from 7.5% to 12.5%. The limits of detection(LOD, S/N≥3) and quantitation(LOQ, S/N≥10) were 0.37~9.55 μg/kg and 1.11~28.65 μg/kg, respectively. Conclusion The real sample tests showed that the proposed method was simple, rapid, sensitive, reliable and cost-effective, and it was suitable for the simultaneous determination of hormones residues in chicken samples

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Objective A multi-residue testing method was developed for the simultaneous determination of 4 androgens, 3 progesterones and 4 glucocorticoids in chicken using QuEChERS sample preparation method with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The homogenized sample extracted with ethyl acetate. The separation was performed on a phenomenex kinetex column by gradient elution after puring from dispersive-solid-phase extraction(d-SPE). The analysis of 11 analytes were operated by electrospray ionization mass spectrometry under the positive or negative mode using multiple reaction monitoring(MRM). Acetonitrile and water(containing 0.1% formic acid) were used as the mobile phase both in positive and negative. Results The correlation coeficients of calibration curves were over 0.991 in the corresponding concentration range. The average recoveries of the 11 analytes at three spiked concentration levels varied from 84.4% to 94.1% and the relative standard deviations(RSDs) varied from 7.5% to 12.5%. The limits of detection(LOD, S/N≥3) and quantitation(LOQ, S/N≥10) were 0.37~9.55 μg/kg and 1.11~28.65 μg/kg, respectively. Conclusion The real sample tests showed that the proposed method was simple, rapid, sensitive, reliable and cost-effective, and it was suitable for the simultaneous determination of hormones residues in chicken samples

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Available abstract

Objective A multi-residue testing method was developed for the simultaneous determination of 4 androgens, 3 progesterones and 4 glucocorticoids in chicken using QuEChERS sample preparation method with ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS). Methods The homogenized sample extracted with ethyl acetate. The separation was performed on a phenomenex kinetex column by gradient elution after puring from dispersive-solid-phase extraction(d-SPE). The analysis of 11 analytes were operated by electrospray ionization mass spectrometry under the positive or negative mode using multiple reaction monitoring(MRM). Acetonitrile and water(containing 0.1% formic acid) were used as the mobile phase both in positive and negative. Results The correlation coeficients of calibration curves were over 0.991 in the corresponding concentration range. The average recoveries of the 11 analytes at three spiked concentration levels varied from 84.4% to 94.1% and the relative standard deviations(RSDs) varied from 7.5% to 12.5%. The limits of detection(LOD, S/N≥3) and quantitation(LOQ, S/N≥10) were 0.37~9.55 μg/kg and 1.11~28.65 μg/kg, respectively. Conclusion The real sample tests showed that the proposed method was simple, rapid, sensitive, reliable and cost-effective, and it was suitable for the simultaneous determination of hormones residues in chicken samples

Key concepts: Chromatography, Quechers, Chemistry, Selected reaction monitoring, Mass spectrometry, Formic acid, Detection limit, Sample preparation

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