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| Rapid Screening and Confirmation of 80 Antibiotic and Hormone Residues in Raw Milk by Ultra Performance Liquid Chromatography-Quadrupole Time of flight Mass Spectrometry |
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| DOI： |
| KeyWord:ultra performance liquid chromatography-quadrupole time of flight mass spectrometry (UHPLC-QTOF MS) raw milk antibiotics hormones rapid screening |
| Author | Institution |
| GONG Song song,ZHANG Jing,YAN Feng,WU Jian ping,PAN Juan,GU Xin |
上海市兽药饲料检测所 |
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| Abstract: |
| A comprehensive analytical method was established for the rapid screening of 80 kinds of antibiotics and hormones in raw milk by ultra performance liquid chromatography-quadrupole time of flight mass spectrometry(UHPLC-QTOF MS)The milk samples were extracted with acetonitrile containing 1% acetic acid.The extracts were cleaned up through QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe) method.80 target compounds were separated on an Agilent ZORBAX SB C18 column(3.0 mm×100 mm，1.8 μm) by gradient elution using acetonitrile-01% formic acid as mobile phases,and detected by MS under Dual AJS ESI+ mode.The analytes were quantified by the matrix-matched calibration standards.As a result,the calibration curves of 80 target compounds were linear in the certain concentration with their correlation coefficients not less than 0990 0.The limits of quantitation (LOQ,S/N=10) for the compounds in milk were in the range of 5-100 μg/kg.The average recoveries for 23 drugs in milk at LOQ spiked levels ranged from 50.2% to 59.7% with their relative standard deviations(RSDs) of 1.1%-13.0%,while those for the other 57 drugs ranged from 61.7% to 119% with their RSDs of 0.3%-19.0%.The screening and confirmation on the analytes were performed by using precision mass,retention time,isotopic abundance and two stage ion mass spectra.The method could be applied in the high throughput screening and identification of antibiotics and hormones in raw milk due to its characteristics of rapidness,simplicity,accuracy and sensitivity. |
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