Simultaneous determination of seventeen glucocorticoids residues in milk and eggs by ultra‐performance liquid chromatography/electrospray tandem mass spectrometry

Abstract

A comprehensive analytical method has been developed and validated for the simultaneous determination of seventeen glucocorticoid residues in eggs and milk. The mass spectrometer parameters, the composition of the mobile phase and the sample preparation method were firstly optimized to obtain maximum sensitivity. The samples were deconjugated with beta-glucuronidase/arylsulfatase enzyme and concentrated using an Oasis HLB solid-phase extraction cartridge, followed by cleanup with a dual Sep-pak silica and aminopropyl cartridge. The analytes were quantified by ultra-performance liquid chromatography (using a C18 column)/electrospray ionization tandem mass spectrometry (UPLC/ESI-MS/MS) operating in the negative ion mode. The assay for the 17 glucocorticoids was linear over the range of 1-200 microg/L for milk and egg samples with a high correlation coefficient (>0.99). The limits of quantification (LOQs) for the target analytes were 0.04-1.27 microg/kg for the egg samples and 0.03-0.73 microg/kg for the milk samples. The average extraction recoveries of the glucocorticoids from eggs and milk at two concentration levels (spiked at 0.40 and 2.00 microg/kg) were 65.6-118.7% and 61.5-119.6%, respectively, with relative standard deviations between 1.8-17.0% and 2.4-18.4%, respectively. Because of its high sensitivity, good precision and specificity, the method was found to be suitable for trace analysis of synthetic and natural glucocorticoids in complex biosamples such as eggs and milk.

Development of a multi-class method for the identification and quantification of residues of antibiotics, coccidiostats and corticosteroids in milk by liquid chromatography–tandem mass spectrometry

“…These values were similar than those reported by other authors (Bohm et al, 2009;Huang, Yuan, & Huang, 2007;Koesukwiwat et al, 2007b) but 10% higher than those reported by Gamba et al (2009) who reported an HPLCeDAD method for the analysis of sulfonamides alone. The lowest recoveries were obtained for the corticosteroids values that were similar to those reported previously (Cui et al, 2006;Stolker et al, 2008). However, recoveries of monensin and salinomycin achieved in milk samples by Stolker et al (2008) were 10 and 22% higher than those achieved in this research.…”

“…Many methods for analysis of antimicrobial agents in food such as sulfonamides, tetracyclines, penicillins have been reported (Cui et al, 2006;Gamba et al, 2009;Hermo, Nemutlu, Kr, Barrón, & Barbosa, 2008;Hoof et al, 2005;Koesukwiwat, Jayanta, & Leepipatpiboon, 2007a;Koesukwiwat et al, 2007b;Li, Wu, Yang, & Zhang, 2010;Marazuela & MorenoBondi, 2004;Ramírez et al, 2003;Volmer, 1996). The tendency nowadays is to develop multi-class methods that permit analysis for a variety of drugs with a single procedure.…”

Fundamental and practical aspects of ultrahigh pressure liquid chromatography for fast separations

“…Due to the efficiency of the 1.7 lm column packing material, the resolution of the test substances was only slightly affected when the linear flow velocity was increased from 0.5 to 1.9 mm/s. Cui et al [106] reported the simultaneous determination of 17 glucocorticoids residues in milk and eggs using UPLC/MS. Because of its high sensitivity, good precision, and specificity, the method was found to be suitable for trace analysis of synthetic and natural glucocorticoids in complex biosamples such as eggs and milk.…”

Three-layer structure graphene/mesoporous silica composites incorporated with C8-modified interior pore-walls for residue analysis of glucocorticoids in milk by liquid chromatography–tandem mass spectrometry

“…These values, which reflect good sensitivity, are substantially lower than the detection limits achieved by LLE [12,21,37]. This method realized wide lineal limit, high sensitivity, precision which are also superior to or comparable with the commercially available columns, such as C18 [17,18], Waters Oasis HLB [16,19,38] and Waters Oasis MCX [20] SPE extraction columns. It was observed Accuracy, LOD and recovery: n = 5. that the method is convenience, sensitive and low consumption of the sample and organic solvents in the pretreated process.…”