Estrogen conjugates in late-pregnancy fluids:  extraction and group separation by a graphitized carbon black cartridge and quantification by high-performance liquid chromatography

Andreolini, Franca; Borra, Claudio; Caccamo, F; Corcia, Antonio Di; Samperi, Roberto

doi:10.1021/ac00140a029

Cited by 85 publications

(51 citation statements)

References 30 publications

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“…Caution must be exercised in the handling of samples since repeated freezing and thawing can cause hydrolysis of conjugates and yield false high values for unconjugated steroids. Thawed specimens are frequently centrifuged to remove precipitates (Leuvering et al, 1983) including precipitated protein (Andreolini et al, 1987;Moneti et a l , 1987).…”

Section: Samples Sampling and Storagementioning

confidence: 99%

“…Indeed, free and total steroid concentrations have been determined by analysis of samples before and after hydrolysis (Axelson et al, 1981;Cartoni and Cocciolo, 1983;Reiffsteck et al, 1982). Clinically, the recent trend has been the determination of a single selected steroid conjugate (Adlercreutz et al, 1975;Stanczyk et al, 1980;Nambara et al, 1985) or all the conjugated forms of a single steroid (Andreolini et al, 1985b;Young et al, 1976Young et al, , 1974Alexander et al, 1979) or the conjugation profile of one class of steroid (Shimada et al, 1986;Fotsis, 1987;Fotsis et al, 1981). In rare cases, both free and conjugated steroids have been determined (Fotsis, 1987;Andreolini et al, 1985b).…”

Section: Recovery Proceduresmentioning

confidence: 99%

“…The choice of a particular system depends on the problem being studied and often, maximum efficiency is attained only by combining techniques (Adlercreutz and Jarvenpaa, 1982;Fotsis, 1987;Fotsis and Adlercreutz, 1987;Risk et al, 1984). Fractionation procedures based on graphitized carbon black (Andreolini et al, 1987;Andreolini et al, 1985b) have been described but have not been widely used.…”

Section: Cleanup and Fractionationmentioning

confidence: 99%

“…However, the efficiencies obtained in ion exchange chromatography have not equalled those obtained with reversed phase materials and ion pair chromatography (Nicolas and LeRoy, 1988;Ager and Oliver, 1984;Shimada et al, 1982a;Slikker el al., 1981;Dixon et al, 1979;Hermansson, 1978;Keravis et al, 1977;Van der Wal and Huber, 1982, 1977 is the preferred method of chromatographing steroid conjugates. For example, Andreolini et al (1987Andreolini et al ( , 1985a have achieved excellent separations of oestrogen sulphates, glucuronates and mixed conjugates as well as free oestrogens on RP-18 packings by eluting with a gradient of acetonitrile + methanol and phosphate buffer containing cetyltrimethylammonium or tetrapropylammonium bromide. The eluant was monitored by fluorescence and UV at either 280 or 215 nm.…”

Section: Stationary Phasementioning

confidence: 99%

“…Indeed, the incidence of bioassays, colorimetric, fluorimetric and radioisotope methods has declined sharply in recent years whereas commercial assay kits (Honjo et al, 1988) have become available for most clinically important steroids. Regardless of the quantification procedure, however, there are many similarities in the preliminary requirements for extraction of steroids, hydrolysis of conjugates and purification of crude extracts, although RIA (McConway and Chapman, 1986) and high performance liquid chromatography (HPLC) (Andreolini et al, 1985a(Andreolini et al, , 1985b can often be applied directly to unmodified samples. Immunochemical procedures offer inherent selectivity but are restricted to single determinations whereas chromatographic procedures such as HPLC offer the combined advantages of sensitivity, accuracy, precision and selectivity together with the ability to perform multiple determinations in a single sample.…”

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confidence: 99%

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Chromatography as a reference technique for the determination of clinically important steroids

Robards

Towers

1990

Biomedical Chromatography

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Chromatographic methods (paper chromatography, thin layer chromatography, high performance liquid chromatography, gas chromatography and gas chromatography-mass spectrometry) for the determination of clinically important steroids in biological specimens are reviewed. The emphasis is on the use of gas chromatography, gas chromatography-mass spectrometry and high performance liquid chromatography as reference rather than routine techniques. Chromatographic methods are compared with colorimetric, fluorimetric and radioimmunoassay procedures in terms of simplicity of operation, cost and ability to analyse large numbers of specimens. The importance of correct specimen collection and storage are discussed. Sample preparation techniques for the various analytical methods are described. These include extraction of free and conjugated steroids from serum, plasma, urine and saliva by solvent partition, with polymer-based resins such as Amberlite XAD-2, DEAE-Sephadex and Sephadex resins bonded with various other function groups and, more recently, with chemically bonded reversed-phase silicas.

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Section: Samples Sampling and Storagementioning

confidence: 99%

Section: Recovery Proceduresmentioning

confidence: 99%

Section: Cleanup and Fractionationmentioning

confidence: 99%

Section: Stationary Phasementioning

confidence: 99%

mentioning

confidence: 99%

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Chromatography as a reference technique for the determination of clinically important steroids

Robards

Towers

1990

Biomedical Chromatography

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Rapid determination of trace nitrophenolic organics in water by combining solid-phase extraction with surface-assisted laser desorption/ionization time-of-flight mass spectrometry

Chen¹,

Shiea²,

Sunner³

2000

Rapid Commun. Mass Spectrom.

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A rapid technique for the screening of trace compounds in water by combining solid-phase extraction (SPE) with activated carbon surface-assisted laser desorption/ionization (SALDI) time-of-flight mass spectrometry is demonstrated. Activated carbon is used both as the sorbent in SPE and as the solid in the SALDI matrix system. This eliminates the need for an SPE elution process. After the analytes have been adsorbed on the surfaces of the activated carbon during SPE extraction, the activated carbon is directly mixed with the SALDI liquid and mass spectrometric analysis is performed. Trace phenolic compounds in water were used to demonstrate the effectiveness of the method. The detection limit for these compounds is in the ppb to ppt range.

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Trace analysis of estrogenic chemicals in sewage effluent using liquid chromatography combined with tandem mass spectrometry

Laganà

Bacaloni

Fago

et al. 2000

Rapid Commun. Mass Spectrom.

106

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A rapid, selective, sensitive, and reproducible method for the analysis of environmental estrogens, either natural or synthetic, present in samples from sewage treatment works (STW) has been developed. Isolation of these compounds from STWs was performed by applying a simple extraction procedure using an ENVI-CARB cartridge (a graphitized non porous carbon black) as the solid-phase extraction (SPE) system. Liquid chromatography coupled with atmospheric pressure chemical ionization (APCI) and tandem mass spectrometry was used for detection. For the multiple reaction monitoring (MRM) mode, the [M + H](+) ion of estrone and the [M + H-H(2)O](+) ions of 17beta-estradiol, estriol and 17alpha-ethynylestradiol were selected as the precursors for collisionally induced dissociation (CID). The average recoveries from sewage final effluent samples ranged from 84 to 93% for low levels, and from 89 to 95% for high levels. The precision of the method ranged from 11 to 8% for low level and from 9 to 7% for high level samples. The lower level of quantitation for these estrogens in STW samples was determined at 0.5 ng/L for 17beta-estradiol and 17alpha-ethynylestradiol, and 1 ng/L for estrone and estriol, based on 1-L aliquots of sewage treatment works water, using the optimum tuning parameters for each individual selected precursor ion/product ion transition. Compared to a previous gas chromatography/mass spectrometry (GC/MS) method for the analysis of ten STW samples, this method was shown to provide higher sensitivity and lower time consumption.

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Estrogen conjugates in late-pregnancy fluids: extraction and group separation by a graphitized carbon black cartridge and quantification by high-performance liquid chromatography

Cited by 85 publications

References 30 publications

Chromatography as a reference technique for the determination of clinically important steroids

Chromatography as a reference technique for the determination of clinically important steroids

Rapid determination of trace nitrophenolic organics in water by combining solid-phase extraction with surface-assisted laser desorption/ionization time-of-flight mass spectrometry

Trace analysis of estrogenic chemicals in sewage effluent using liquid chromatography combined with tandem mass spectrometry

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