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| Determination of Eleven β-Blocker Residues in Animal Derived Foods by Ultra High Performance Liquid Chromatography-Tandem Mass Spectrometry with Molecularly Imprinted Solid Phase Extraction |
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| DOI： |
| KeyWord:molecularly imprinted solid phase extraction liquid chromatography-tandem mass spectrometry (LC-MS/MS) β-blocker residue determination |
| Author | Institution |
| HAO Jie，JIANG Jie，SHAO Rui-ting，DING Xue-yan，SHI Na，LU Yong |
北京市食品安全监控和风险评估中心 |
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| Abstract: |
| A molecularly imprinted solid phase extraction coupled with ultra high performance liquid chromatography-tandem mass spectrometric (UPLC-MS/MS) method was developed for the determination of eleven beta blocker residues in animal derived foods.The sample was enzymed with β-glucuronidase/aryl sulfatase.The supernatant fraction was adjusted to the optimal pH value，and then extracted with isopropanol-ethyl acetate (5∶5，by volume).The organic solvent was first evaporated to dryness, and then redissolved，finally purified by molecularly imprinted solid phase extraction.The analyte was separated with a BEH C18 column by gradient elution using methanol-5 mmol/L ammonium acetate (containing 0.1% formic acid) as mobile phase，and detected by MS under ESI+ ionization and multiple reactions monitoring mode.The quantification of the analytes was performed by the matrix standard addition method.The limits of detection and limits of quantitation were in the ranges of 0.02-0.1 μg/kg and 0.05-0.25 μg/kg，respectively.The calibration curves of 11 β-blockers were linear in the range of 0.05- 10 μg/kg，with correlation coefficients not less than 0.991.Under three spiked levels，the average recoveries of the analytes in pork and liver were 73.2%-108.3% and 70.2%-98.2%，respectively，with relative standard deviations of 1.3%-9.5% and 3.7%-9.8%，respectively.The method is rapid，sensitive and precise，and is suitable for the determination of β-blocker multi residues in animal derived foods. |
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