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| Simultaneous and Rapid Screening of 39 Prohibited Drugs in Horse Feed Using Liquid Chromatography-Tandem Mass Spectrometry |
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| DOI：10.3969/j.issn.1004-4957.年份.月份 |
| KeyWord:LC-MS/MS horse feed equine dopings fast screening |
| Author | Institution |
| 高照，吴侔天，曹建民 |
1.中国反兴奋剂中心;2.北京体育大学运动人体科学学院 |
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| Abstract: |
| A high-throughput liquid chromatography-tandem mass spectrometric(LC-MS/MS) method was established for the simultaneous screening of 39 drugs for horse racing in horse feed prohibited by the International Equestrian Federation(IEF)，including opiod analgesics，antimalarial，antispasmodic，antiarrhythmic，anticonvulsant，stimulants and psychotropic drugs.Feed samples were deproteinated and extracted with 1 mmol/L HClO4 for the basic drugs and then with acidified acetonitrile in 20 min by sonication.The purification was performed by mix-mode solid-phase extraction(SPE) using multi-step loading of the extracts in weak acid and organic solutions and multi elute with dichloromethane-isopropanol-concentrated aqueous ammonia(5∶4∶1) and acetonitrile.The extracts were separated on an Agilent Zorbax SB（10.0 cm×2.1 mm i.d.，3.5 μm） column with 0.4% formic acid and 0.4% formic acid acetonitrile solution as mobile phase by gradient elution and analyzed by LC-MS/MS under positive electro-spray ionization(ESI+)mode with multiple reaction monitoring(MRM)mode.The method was validated with fortified samples at three levels and the results showed that the recoveries were in the range of 58%-116% with relative standard deviations of 1.6%-20.4%.The limits of detection（LODs,S/N≥3) and limits of quantitation（LOQs,S/N≥10)were 0.2-25.0 μg/kg and 1.0-40.0 μg/kg，respectively,among which more than 67% LODs of the drugs analyzed were below 25 μg/kg.This method has the advantages of saving time, good selectivity and sensitivity，and can be applied in the screening and confirmation of the drugs mentioned above in horse feed in routine analysis. |
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