Determination of endogenous and synthetic glucocorticoids in human urine by gas chromatography–mass spectrometry following microwave-assisted derivatization

Amendola, Luca; Garribba, Flaminia; Botrè, Francesco

doi:10.1016/s0003-2670(03)00703-7

Cited by 92 publications

(50 citation statements)

References 22 publications

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“…In this study, three kinds of sex hormones were simultaneously determined instead of only one kind of specific sex hormone in some literature [27,30,32,33]. Some parameters affecting the MAD, such as derivatization time, microwave power, and reaction solvent, were investigated.…”

Section: Optimization Of Mad Conditionsmentioning

confidence: 99%

“…In recent years, microwave-accelerated derivatization (MAD) has become an alternative and powerful technique for the derivatization of some compounds [26][27][28][29][30][31][32][33][34][35]. Derivatization reaction using microwave dielectric heating can not only reduce analysis time but also produce comparable to or higher yields than TTD.…”

Section: Introductionmentioning

confidence: 99%

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Microwave‐accelerated derivatization prior to GC‐MS determination of sex hormones

Zhao

Zhang

et al. 2011

J of Separation Science

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A new microwave-accelerated derivatization method was developed for rapid determination of 13 natural sex hormones in feeds. Sex hormones were isolated from the sample matrix by ultrasonic extraction, followed by solid-phase extraction, derivatized under microwave irradiation, and then analyzed directly by gas chromatography-mass spectrometry (GC-MS) in selective ion monitoring (SIM) mode. The key parameters affecting derivatization efficiency, including microwave irradiation time, microwave power, and reaction solvent were studied. Under microwave power of 360 W and microwave irradiation for 3 min, 13 natural sex hormones were simultaneously derivatized using heptafluorobutyric acid anhydride (HFBA) as derivatization reagent. This method was applied to the determination of 13 natural sex hormones in different feed samples, and the obtained results were compared with those obtained by the traditional thermal derivatization. The recoveries from 58.1 to 111% were obtained at sex hormone concentrations of 10-300 μg/kg with RSDs ≤12.0%. The results showed that the proposed method was fast, simple, efficient and can be applied to the determination of 13 natural sex hormones in different feed samples.

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Section: Optimization Of Mad Conditionsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Microwave‐accelerated derivatization prior to GC‐MS determination of sex hormones

Zhao

Zhang

et al. 2011

J of Separation Science

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“…However, with DAD detection, the detection limit can not meet the requirements by legislation (0.5 MRL), and the chromatographic peaks of dexamethasone and betamethasone can not be isolated in the chromatogram. On the other hand, GC-MS [15,16] is not preferable due to the involvement of tedious derivatization sample preparation steps. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) [17][18][19][20][21][22][23] provides a rapid, accurate and sensitive alternative to detect such residues.…”

Section: Introductionmentioning

confidence: 99%

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

Liu

Feng

Sun

et al. 2015

Analytica Chimica Acta

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“…Gas chromatography-mass spectrometry (GC-MS) [8,9], liquid chromatography-mass spectrometry (LC-MS/MS) [4,10] and methods based on immunoaffinity chromatography followed by reverse-phase highperformance liquid chromatography (IAC-HPLC) with diode array detection (DAD) [2] have been developed to identify corticosteroids in biological samples. In recent years, liquid chromatography coupled to different massspectrometry detectors has become a frequently used to quantitatively determine corticosteroids in complex matrices [10][11][12].…”

Section: Introductionmentioning

confidence: 99%

Evaluation of Molecularly Imprinted Polymers for the Simultaneous SPE of Six Corticosteroids in Milk

et al. 2012

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A molecularly imprinted solid-phase extraction procedure was optimized for the simultaneous extraction of six corticosteroids commonly employed in animal husbandry. Two different molecularly imprinted polymers (MIPs) were synthetized by precipitation polymerization, using dexamethasone (DM) and flumethasone (FLU) as template molecules. Methacrylic acid was used as functional monomer and divinylbenzene as cross-linker, and the selected porogen was a solution of acetonitrile and toluene (3:1). After removal of the template, both molecularly imprinted and non-imprinted polymers were placed into glass cartridges to perform solid-phase extraction experiments. Loading, washing and elution steps were optimized for each MIP in order to test the suitability of the selected template molecules DM and FLU to provide selective polymeric sites for corticosteroids. Recovery measurements were performed by HPLC-MS/MS. The maximum recovery for all corticosteroids was achieved with DMbased MIP when loading with toluene and washing with 5% acetonitrile in toluene, and eluting with 1% acetic acid in methanol. When cleaning-up milk samples spiked with corticosteroids, the recovery of DM-based polymer decreased. However, the efficiency of FLU-based polymer clearly improved even when a strong matrix effect was observed. Additionally, two frequently used commercial solid-phase extraction (SPE) cartridges were compared with imprinted polymers. The commercial SPE cartridges gave good recoveries only for specific analytes while MIPs provided good recoveries for all analyzed corticosteroids.

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Determination of endogenous and synthetic glucocorticoids in human urine by gas chromatography–mass spectrometry following microwave-assisted derivatization

Cited by 92 publications

References 22 publications

Microwave‐accelerated derivatization prior to GC‐MS determination of sex hormones

Microwave‐accelerated derivatization prior to GC‐MS determination of sex hormones

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

Evaluation of Molecularly Imprinted Polymers for the Simultaneous SPE of Six Corticosteroids in Milk

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