PMID- 9323541 OWN - NLM STAT- MEDLINE DCOM- 19971120 LR - 20190831 IS - 1387-2273 (Print) IS - 1387-2273 (Linking) VI - 696 IP - 2 DP - 1997 Aug 29 TI - Quantitative determination of several synthetic corticosteroids by gas chromatography-mass spectrometry after purification by immunoaffinity chromatography. PG - 203-15 AB - A study was conducted to test a multiresidue analytical procedure for detecting and quantifying several corticosteroids on which the European Union imposes maximum residue limits (MRLs). Primary extracts from different matrices (liver, milk, urine, faeces) were first purified on C18 cartridges. A new immunoaffinity clean-up step was included. The immunoaffinity gel was used to purify several corticosteroids simultaneously with enrichment of the corresponding fractions. The extracts were treated with an aqueous solution of pyridinium chlorochromate to fully oxidise all corticosteroids and to facilitate their extraction with dichloromethane. After evaporation, the final extract was reconstituted with toluene before injection into the GC-MS apparatus. The analysis was performed in the CI-negative ionisation mode using ammonia as the reactant gas. The estimated detection and quantification limits were, respectively, 0.25 and 0.5 ppb or lower. Overall, the method is reproducible to within 20%. Recovery is between 50 and 80% according to the corticosteroid. FAU - Delahaut, P AU - Delahaut P AD - CER, Laboratoire d'Hormonologie, Marloie, Belgium. FAU - Jacquemin, P AU - Jacquemin P FAU - Colemonts, Y AU - Colemonts Y FAU - Dubois, M AU - Dubois M FAU - De Graeve, J AU - De Graeve J FAU - Deluyker, H AU - Deluyker H LA - eng PT - Journal Article PL - Netherlands TA - J Chromatogr B Biomed Sci Appl JT - Journal of chromatography. B, Biomedical sciences and applications JID - 9714109 RN - 0 (Adrenal Cortex Hormones) SB - IM MH - Adrenal Cortex Hormones/*analysis/isolation & purification MH - Animals MH - Cattle MH - Chromatography, Affinity/*methods MH - Feces/chemistry MH - Gas Chromatography-Mass Spectrometry/*methods MH - Liver/chemistry MH - Mass Spectrometry MH - Milk/chemistry MH - Reference Standards MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Urine/chemistry EDAT- 1997/08/29 00:00 MHDA- 1997/11/05 00:01 CRDT- 1997/08/29 00:00 PHST- 1997/08/29 00:00 [pubmed] PHST- 1997/11/05 00:01 [medline] PHST- 1997/08/29 00:00 [entrez] AID - 10.1016/s0378-4347(97)00222-3 [doi] PST - ppublish SO - J Chromatogr B Biomed Sci Appl. 1997 Aug 29;696(2):203-15. doi: 10.1016/s0378-4347(97)00222-3.