A gas-liquid chromatographic assay of melatonin and indoleamines using heptafluorobutyryl derivatives

Degen, P.H.; DoAmaral, Jefferson R.; Barchas, Jack D.

doi:10.1016/0003-2697(72)90225-4

Cited by 30 publications

(6 citation statements)

References 6 publications

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“…In these studies, intact indoleamines [15,17,18], acetylated derivatives [16], and trimethylsilyl and trifluoroacetyl derivatives ( [19]. Later, the application of gas chromatography-mass spectrometry (GC/MS) led to the quantitative analysis of Mel [20][21][22][23][24][25][26], 5HT [21][22][23]27], MTPL [24][25][26], 5MT [21,22,27], and MIAA [26] in the pineal gland [20][21][22][24][25][26] and hypothalamus [21,22,27]. Appropriate derivatization of Mel and other indoleamines gives them adequate vapor pressure for gas chromatography.…”

Section: Gas Chromatography and Gas Chromatography-mass Spectrometrymentioning

confidence: 99%

“…Appropriate derivatization of Mel and other indoleamines gives them adequate vapor pressure for gas chromatography. Derivatization of authentic Mel and biogenic samples were performed with a silanizing agent to form trimethylsilyl melatonin (TMS-Mel) [24,25], with heptafluorobutyrylimidazole to form diheptafluorobutyryl melatonin (HFB-Mel) [20], or with pentafluoropropionic anhydride to form pentafluoropropionyl melatonin (PFP-Mel) [21][22][23]26,27]. Fig.…”

Section: Gas Chromatography and Gas Chromatography-mass Spectrometrymentioning

confidence: 99%

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Separation and assay methods for melatonin and its precursors

Harumi

Matsushima

2000

Journal of Chromatography B: Biomedical Sciences and Applicatio

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ELSEVIER, Harumi, T; Matsushima, S, JOURNAL OF CHROMATOGRAPHY. B, BIOMEDICAL AND APPLICATIONS, 747(1-2), 95-110, 2000. authorMelatonin is an indoleamine hormone that is synthesized from tryptophan via 5-hydroxytryptophan, serotonin and N-acetylserotonin in the vertebrate pineal gland. Many chromatographic and non-chromatographic techniques have been developed and improved for the determination and measurement of melatonin and its related indoleamines. At present, gas chromatography with mass spectrometry and reversed-phase high performance liquid chromatography with fluorescence or electrochemical detection are widely used for indoleamine determinations in the pineal gland. This review will deal with methods for the separation and determination of the melatonin and its related indoleamines

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Section: Gas Chromatography and Gas Chromatography-mass Spectrometrymentioning

confidence: 99%

Section: Gas Chromatography and Gas Chromatography-mass Spectrometrymentioning

confidence: 99%

Separation and assay methods for melatonin and its precursors

Harumi

Matsushima

2000

Journal of Chromatography B: Biomedical Sciences and Applicatio

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“…Many methods for the detection of melatonin in body fluids have been reported, such as high performance liquid chromatography (HPLC) coupled to fluorescence detector [28], gas chromatography mass spectrometry (GC-MS) [29,30], HPLC-LC/MS [31,32], capillary electrophoresis [33], radioimmunoassay (RIA) [34], enzyme-linked immunosorbent assay (ELISA) [35,36], colorimetric sensor arrays [37][38][39]. Among them, ELISA kit for detection of melatonin is commercially available and the LOD was 0.5 pg mL −1 [40].…”

Section: Introductionmentioning

confidence: 99%

Simple Colorimetric and Fluorometric Assay Based on 2,3-Naphthalenedialdehyde for Melatonin in Human Saliva

et al. 2019

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In this paper, 2,3-naphthalenedialdehyde (2,3-Nda) was selected as color reagent with colorimetric and fluorometric assay for detecting melatonin in human saliva. 2,3-naphthalenedialdehyde reacted with melatonin under the catalysis of hydrochloric acid and Fe 3+ , which the color change was observed sensitively from colorless to yellow with the naked eye. On the other hand, the product of the reaction had a large conjugate structure with strong fluorescence for the fluorometric analysis. Under optimized experimental conditions, a concentration range of melatonin was 2.5-37.5 µM (R 2 = 0.998) by colorimetry with the limit of detection for 1.288 µM (S/N = 3), and 0.01-0.1 µM (R 2 = 0.997) by fluorometry with the limit of detection for 0.004 µM (S/N = 3). The two assays were successfully applied to the determination of melatonin in human saliva, which average recoveries were 97.80% and 95.96%, respectively, which has the potential in fast clinical examination of melatonin in human saliva.

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“…Gas chromatography-mass spectrometry (GC-MS) detection of melatonin requires sample derivatization for melatonin volatilization by, for example, the use of pentafluoropropionic anhydride or heptafluorobutyrylimidazole [70, 71]. In another approach, human plasma samples have been directly injected into and evaluated in an HPLC system with fluorescence detection without prior extraction or purification, achieving a detection limit of 1 ng per ml of human plasma (4 pmol/ml) [72].…”

Section: Introductionmentioning

confidence: 99%

Measurement of melatonin in body fluids: Standards, protocols and procedures

et al. 2010

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Background and PurposeThe circadian rhythm of melatonin in saliva or plasma, or of the melatonin metabolite 6-sulfatoxymelatonin (a6MTs) in urine, is a defining feature of suprachiasmatic nucleus (SCN) function, the body’s endogenous oscillatory pacemaker. The primary objective of this review is to ascertain the clinical benefits and limitations of current methodologies employed for detection and quantification of melatonin in biological fluids and tissues.Data IdentificationA search of the English-language literature (Medline) and a systematic review of published articles were carried out.Study SelectionArticles that specified both the methodology for quantifying melatonin and indicated the clinical purpose were chosen for inclusion in the review.Data ExtractionThe authors critically evaluated the methodological issues associated with various tools and techniques (e.g. standards, protocols, and procedures).Results of Data SynthesisMelatonin measurements are useful for evaluating problems related to the onset or offset of sleep and for assessing phase delays or advances of rhythms in entrained individuals. They have also become an important tool for psychiatric diagnosis, their use being recommended for phase typing in patients suffering from sleep and mood disorders. Additionally, there has been a continuous interest in the use of melatonin as a marker for neoplasms of the pineal region. Melatonin decreases such as found with aging are or post pinealectomy can cause alterations in the sleep/wake cycle. The development of sensitive and selective methods for the precise detection of melatonin in tissues and fluids has increasingly been shown to have direct relevance for clinical decision making.ConclusionsDue to melatonin’s low concentration, as well as the coexistence of numerous other compounds in the blood, the routine determination of melatonin has been an analytical challenge. The available evidence indicates however that these challenges can be overcome and consequently that evaluation of melatonin's presence and activity can be an accessible and useful tool for clinical diagnosis.

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A gas-liquid chromatographic assay of melatonin and indoleamines using heptafluorobutyryl derivatives

Cited by 30 publications

References 6 publications

Separation and assay methods for melatonin and its precursors

Separation and assay methods for melatonin and its precursors

Simple Colorimetric and Fluorometric Assay Based on 2,3-Naphthalenedialdehyde for Melatonin in Human Saliva

Measurement of melatonin in body fluids: Standards, protocols and procedures

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