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KMID : 0385520090220040326
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Analytical Science & Technology
2009 Volume.22 No. 4 p.326 ~ p.335
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Simultaneous analysis of residual glucocorticoids in egg by LC/MS/MS
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Jang Mi-Ae
Myung Seung-Woon
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Abstract
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A specific analytical method able to identify and quantify traces of six glucocorticoids residues in eggs were developed. The extraction and clean-up parameters for simultaneous analysis were evaluated and HPLC and spectrometric conditions were also established. For determination of glucocorticoids, 5 g of egg was transferred into a test tube, adjusted pH 5.2 with acetate buffer and was β-glucuronidase/arylsulfatase from Helix pomatia added. The mixture was centrifuged and supernatant was extracted twice with 20 mL n-hexane. The extraction was performed with HLB cartridge using methanol, followed by clean-up with silica cartridge using methanol/ethyl acetate (4/6, v/v). The analytes were determined by HPLC/ESI-MS/MS operating in the negative ion mode. Validation studies with fortified egg samples for established method were performed. The result of method validation gave good efficiency, linearity, accuracy and precision. The correlation coefficients (r²) of the calibration curves appeared to be higher than 0.99 in egg, indicating excellent linearity. LOD was ranged 0.09 to 0.17 ㎍/㎏, and recoveries for most compounds were in the range of 55.7-69.8%. This method can be used to determine ㎍/㎏ levels of glucocorticoids in eggs.
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KEYWORD
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Glucocorticoids, LC/MS/MS, egg
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