Response Surface Optimization of the QuEChERS Combined with UHPLC-MS/MS Method for Determination of Tetracyclines in Muscle of Channa argus
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LI Lichun,
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LIU Shugui,
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LIN Jiawei,
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YIN Yi,
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ZHENG Guangming,
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ZHAO Cheng,
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MA Lisha,
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SHAN Qi,
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DAI Xiaoxin,
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WEI Linting,
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ZHOU Hao
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Graphical Abstract
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Abstract
A quick, easy, cheap, effective, rugged and safe pre-treatment method (QuEChERS) was established to evaluate the risk of tetracycline residues in the muscle of Channa argus. The Box-Behnken design (BBD) response surface optimization method was used to optimize the extraction and purification conditions. The samples were extracted with 10 mL acetonitrile (containing 1% formic acid) and 2 mL 0.1 mol/L Na2EDTA-Mcllvaine buffer solution, and the extracts were purified by 150 mg primary secondary amine(PSA)and 200 mg C18, and detected with Ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The result showed that the calibration curve was linear in the range of 0.50~100 ng/mL, with high correlation coefficients (r≥0.999). The limits of detection (LOD) and quantification (LOQ) were 0.25~0.75 μg/kg and 0.84~2.00 μg/kg, respectively. The average recoveries of tetracycline, oxytetracycline, chlortetracycline and doxycycline at three different spiked levels in the muscle of Channa argus were 89.5%~118%, with relative standard deviations (RSDs) of 1.11%~8.88%. This method is simple, sensitive and accurate, and can be used for the rapid quantitative determination of tetracyclines in Channa argus.
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