by Ultra High-performance Liquid
Chromatography/Tandem Mass Spectrometry
島津評論 69〔1・2〕 165～172 (2012.9)
A method for determining seven glucocorticoids（prednisone, prednisolone, hydrocortisone, dexamethasone,beclomethasone, methylprednisolone, and fl udrocortisone acetate）in milk powder using a Shimadzu LC-30A ultra high-performance liquid chromatograph coupled with an LCMS-8030 triple quadrupole mass spectrometer was established. Rapid separation and detection of glucocorticoids were completed within 2 minutes. Excellent linearity（the correlation coeffi cients above 0.999）within the concentration range of 0.5～40μg/L were obtained.
In precision experiments performed with mixed standard solutions at 2μg/L, 10μg/L and 40μg/L, the relative standard deviations of the retention time and peak area of 6 successive injections were below 0.6 ％ and 3.9 ％,respectively. Accuracies at 2μg/L, 10μg/L and 40μg/L ranged between 80.4 ％ and 105.4 ％. The limit of quantitation for prednisone, prednisolone, hydrocor tisone, dexamethasone, beclomethasone and methylprednisolone was 0.4μg/kg, and that for fl udrocortisone acetate was 1.0μg/kg. Those results indicate the method meets the requirements in the China official method “GB/T 21981-2008 Method for determination of hormone residues in animal derived food by liquid chromatography-tandem mass spectrometry”.
Keywords : Glucocorticoids, Milk powder, Ultra high-performance liquid chromatograph, Triple quadrupole mass spectrometer
1Shimadzu Global COE for Application & Technical Development, Shimadzu (China) Co., Ltd., Shanghai, China