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| Determination of 25 Glucocorticoids in Milk by Ultra-performance Liquid Chromatography - Tandem Mass Spectrometry with Nanofiber Solid Phase Extraction |
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| DOI： |
| KeyWord:glucocorticoids nanofiber solid phase extraction polystyrene ultra-performance liquid chromatography - tandem mass spectrometry milk |
| Author | Institution |
| WU Xiao-xiao，JIANG Di-yao，MEI Xiu-ming，KANG Xue-jun，LI Yu-feng1，ZHANG Chi |
1. Key Laboratory of Biotoxin Analysis & Assessment for State Market Regulation，Nanjing Institute of Product Quality Inspection，Nanjing ，China; 2. School of Biological Science & Medical Engineering， Southeast University，Nanjing ，China |
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| Abstract: |
| A novel ultra-performance liquid chromatography - tandem mass spectrometry（UPLC - MS/MS） with polystyrene（PS） nanofiber solid phase extraction was developed for the simultaneous determination of 25 glucocorticoids in milk after the optimization of chromatographic and extraction conditions. The PS nanofiber was prepared by electrostatic spinning，then characterized by scanning electron microscopy， transmission electron microscopy and infrared spectroscopy. Subsequently， the BET surface area and contact angle of the PS nanofiber were measured. The milk sample was extracted using vortex mixer with acetonitrile. The analytes were concentrated and purified with the PS nanofiber solid phase extraction column. The chromatographic separation of the methanol eluent was performed on an ACQUITY BEH C18 （2.1 mm × 100 mm，1.7 μm） column by gradient elution，with 0.1% formic acid aqueous solution and acetonitrile as mobile phases. The analysis was performed by mass spectrometry with jet stream electrospray ionization in positive mode under multiple reaction monitoring（MRM） mode. The analytes were quantified by external standard method. Results of the method validation showed that there were good linear relationships for 25 glucocorticoids in the concentration range of 1 - 100 μg/L，with their correlation coefficients（r） larger than 0.995.The limits of detection（LOD，S/N ≥ 3） and limits of quantitation（LOQ，S/N ≥ 10） for 25 glucocorticoids were in the range of 0.04 - 0.10 μg/kg and 0.13 - 0.33 μg/kg，respectively. The recoveries for 25 glucocorticoids in the spiked sample at three concentration levels ranged from 71.5% to 105%，with relative standard deviations（RSDs） of 1.8% - 10%. The established method is simple，rapid，accurate and sensitive. The method was applied to detect 25 glucocorticoids in 10 batches of milk samples. Only one of them were found to contain trace hydrocortisone residue. |
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