High-performance liquid chromatographic determination of 3α,5β- tetrahydroaldosterone in human urine with chemiluminescence detection

Ishida, Junichi; Sonezaki, Shinji; Yamaguchi, Masatoshi; Yoshitake, Takashi

doi:10.1039/an9921701719

Cited by 18 publications

(9 citation statements)

References 21 publications

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“…Chemiluminiscence (CL) has been proposed by other workers (10)(11)(12)(13) for the detection of corticosteroids, but in most of those cases prior derivatization with different compounds is mandatory. In previous works, the CL reaction produced by natural and synthetic corticosteroids when reacting with luminol in the presence of a catalyst [hexacyanoferrate (III)] in alkaline solution was studied under both static (6) and dynamic (7,14) conditions.…”

Section: Resultsmentioning

confidence: 99%

Detection of synthetic corticosteroids in bovine urine by chemiluminescence high‐performance liquid chromatography

Vázquez¹,

Feás²,

Lolo³

et al. 2005

Luminescence

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The development of a black market of chemical cocktails for illegal growth promotion in food-producing animals includes substances that are potentially dangerous for human health, such as synthetic corticosteroids. The potential presence of these residues in food makes it necessary to develop rapid and sensitive analytical methodologies to detect such substances, preferably in live animals before they arrive at the market. A chemiluminescence (CL) detection method for the determination of four synthetic corticosteroids (prednisolone, betamethasone, dexamethasone and flumethasone) in bovine urine has been developed. The proposed system, which does not need any derivatization procedure, offers an easy method well suited for routine research. Urine samples were homogenized with methanol:water (50:50, v/v) and centrifuged. The upper layer was collected and Strata X cartridges were used for cleaning up. The purified residues were evaporated to dryness and then redissolved in the mobile phase. Analysis of the extracts was performed using high-performance liquid chromatography with chemiluminescence detection, employing luminol as the CL reagent. The recovery curves, obtained at four spiking levels (different for each corticosteroid), showed that recoveries of at least 70% could be obtained for urine. The chemiluminescence detection procedure afforded satisfactory results with respect to sensitivity and the LOD and LOQ, taken as the first point of the regression curve, ranged from 4 ppb to 65 ppb. The maximum mean RSD was below 13% and below 15% for intra- and inter-day assay, respectively, in all cases.

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Section: Resultsmentioning

confidence: 99%

Detection of synthetic corticosteroids in bovine urine by chemiluminescence high‐performance liquid chromatography

Vázquez¹,

Feás²,

Lolo³

et al. 2005

Luminescence

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“…This method was also employed in the determination of N-acetylneuraminic acid in human serum and urine (Ishida et al, 1992b). Dexamethasone and 3a,5b-tetrahydroaldosterone were detected after the conversion of their keto group to adicarbonyl group by the reaction with copper(II) acetate, and the derivatization of the resultant glyoxal compounds with DPH (Ishida et al, 1992c(Ishida et al, , 1993.…”

Section: Luminol CL Detectionmentioning

confidence: 99%

Chemiluminescence detection in HPLC and CE for pharmaceutical and biomedical analysis

Li¹,

Zhang²,

Guo³

et al. 2003

Biomedical Chromatography

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The present paper reviews the developments and applications of chemiluminescence detection with HPLC and CE in pharmaceutical and biomedical analysis. The chemiluminescence systems, chemiluminogenic reagents and derivatization reagents, improvements in instrumental design as well as their contributions to the practical applications, are all presented. The advantages and limitations of current detection methodology and future prospects for improvement are briefly discussed.

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“…The resulting optimum conditions were quite similar to those described previously. 13 The peak heights of DPH derivatives for dexamethasone and beclomethasone in the final mixture did not change for at least 5 h in daylight at room temperature.…”

Section: Hplc Conditionsmentioning

confidence: 99%

“…The oxidation conditions were the same as those described by Gorog and Szepesil' and Yamaguchi et al '8 The chemiluminescence derivatization conditions for 3a,5$-tetrahydroaldosterone and aldosterone were described previously. 13 In this study, the conditions for dexamethasone and beclomethasone were examined. The resulting optimum conditions were quite similar to those described previously.…”

Section: Hplc Conditionsmentioning

confidence: 99%

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Determination of Dexamethasone in Plasma by High-Performance Liquid Chromatography with Chemiluminescence Detection

et al. 1993

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KeywordsHigh-performance liquid hydrazide, plasma chromatography, dexamethasone, chemiluminescence, 4,5-diaminophthalDexamethasone, 9a-fluoro-16a-methyl-1 1f3,17a,21-trihydroxy-l,4-pregnadiene-3,20-dione, is a synthetic corticosteroid which has been widely used for the treatment of various kinds of diseases such as endocrinopathy, rheumatism and nephrotic syndorome owing to its anti-allergic and anti-inflammatory actions. Because dexamethasone has strong efficacy against the diseases, the dose of the drug is much smaller (several mg per day) than those of other synthetic corticosteroids. Therefore, a sensitive method is required for the determination of dexamethasone in plasma after administration for efficient and safety use of the drug.Several methods involving radioimmunoassay (RIA)1-3, gas chromatography-mass spectrometry (GC-MS)4 and liquid chromatography (LC)s-12 have been reported for the determination of dexamethasone in plasma/serum. Although the RIA methods are very sensitive, they require chromatographic purification to avoid crossreaction with other endogeneous corticosteroids. The GC-MS method needs a relatively complicated procedure for sample pretreatment. Spectrophotometric LC5-11 are not very sensitive and thus require a large amount of plasma (2 -3 ml). A fluorometric LC12, which involves precolumn derivatization with 9-anthroylnitrile, is fairly sensitive. However, the method requires solidphase extraction cartridges for the clean-up of plasma and the elimination of the excess reagent before and after the derivatization.We have previously reported a chemiluminometric LC method13 for the determination of 3a,5/3-tetrahydroaldosterone in human urine. The method is based on the conversion of the corticosteroid into the corresponding glyoxal compound by copper(II) acetate oxidation. The glyoxal compound is derivatized with 4,5-diaminophthalhydrazide (DPH), a chemiluminescence derivatization reagent for a-dicarbonyl compounds14, to yield a chemiluminescent quinoxaline. The resulting quinoxaline produces chemiluminescence by reaction with hydrogen peroxide in the presence of potassium hexacyanoferrate(III) in alkaline medium after LC separation.Recently, it was found that dexamethasone generates chemiluminescence by the same derivatization and chemiluminescence reactions as described above. Our present objective is to develop a sensitive and selective LC method involving a simple pretreatment of plasma samples by precolumn Chemiluminescence derivatization with DPH for the quantification of dexamethasone in plasma. Beclomethasone (9a-chloro-16/3-methyl-1 1f3,17a,21-trihydroxy-l,4-pregnadiene-3,20-dione), which has a structure similar to that of dexamethasone, was used as an internal standard for the precise determination of dexamethasone.Dexamethasone concentrations in plasma from a healthy volunteer after oral administration of dexamethasone were measured by the established method.

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High-performance liquid chromatographic determination of 3α,5β- tetrahydroaldosterone in human urine with chemiluminescence detection

Cited by 18 publications

References 21 publications

Detection of synthetic corticosteroids in bovine urine by chemiluminescence high‐performance liquid chromatography

Detection of synthetic corticosteroids in bovine urine by chemiluminescence high‐performance liquid chromatography

Chemiluminescence detection in HPLC and CE for pharmaceutical and biomedical analysis

Determination of Dexamethasone in Plasma by High-Performance Liquid Chromatography with Chemiluminescence Detection

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