Development and validation of a high performance liquid chromatography assay for 17α-methyltestosterone in fish feed

Marwah, Ashok; Marwah, Padma; Lardy, Henry A.

doi:10.1016/j.jchromb.2005.07.005

Cited by 23 publications

(21 citation statements)

References 14 publications

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“…3 (1): 1-9 (2011) , 2004). We have earlier studied degradation of MT under accelerated stress situations at high and low pH (Marwah et al 2005). Selected samples from aerobic and anaerobic experiments were subjected to LC-MS analysis under scan mode and data subjected to the extracted ion analysis for the expected degradation products.…”

Section: Resultsmentioning

confidence: 99%

“…The sediment remaining in the original incubation vessels was stored frozen at -40°C until analysis. Analytical methods Water extraction:The quantity of MT in water samples was determined using LC-MS method reported earlier (Marwah et al, 2010). In short, twenty-five ml of test water from each incubation in the aerobic and anaerobic trials was used for analysis.…”

Section: Mt (I) Is (Ii)mentioning

confidence: 99%

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Transformation of 17a-methyltestosterone in aquatic-sediment systems

Barry

Marwah

2011

JANS

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Abstract:Two sediment samples that differed with respect to total organic carbon and texture ("sand" and "clay") were exposed to radio inert 17α-methyltestosterone (MT) or [14 C]-radiolabeled 17α-methyltestosterone ( 14 C-MT), under both aerobic and anaerobic conditions, for up to 56 days, to characterize the fate of MT in the aquatic environment. Radio inert MT was quantified by a highly sensitive liquid chromatography/mass spectrometry (LC-MS) method and radioactive MT was quantified by HPLC using an in-line flow liquid scintillation counter (LSC). The data suggest that MT entering the aquatic environment is converted into metabolites that become tightly associated with the sediment. Half-lives for MT dissipation in the sediment systems ranged from 2-9 days, depending on the sediment type and the presence of oxygen. Sediment type had little effect on MT dissipation. The mineralization of MT under aerobic conditions was low (<9% conversion of MT to CO 2 ).

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Section: Resultsmentioning

confidence: 99%

Section: Mt (I) Is (Ii)mentioning

confidence: 99%

Transformation of 17a-methyltestosterone in aquatic-sediment systems

Barry

Marwah

2011

JANS

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“…Estrogens and Androgens, Dehydroepiandrosterone and its metabolites, Pregnanes and active Corticosteroids were found not to interfere in the present assay. Specifically the following hormones and steroids were studied for interference, and were found not to interfere with the present assay: Testosterone; Androst-5-en-3,17-dione; DHEA (Dehydroepiandrosterone); Androstenediol (Androst-5-en-3β,17β-diol); 7-oxo-DHEA; 7α-OH DHEA; 7β-OH DHEA; 16α-OH DHEA; 7β-AET (Androst-5-en-3β,7β,17β-triol); 7α-AET (Androst-5-en-3β,7α,17β-triol); 7-oxo-Diol (3β,17β-dihydroxyandrost-5-en-7-one); Estrone; Estradiol; Estriol; Progesterone; Pregnenolone; Cortisol; Cortisone; Cortexolone; Cortexone; Dehydrocorticosterone; Corticosterone; and 17α-OH Pregnenolone (Table 3); and iv) by subjecting MT to degradation studies at low, neutral, and high pH at elevated temperature (Marwah et al, 2005). LC-MS analysis of MT samples subjected to accelerated stress study showed no interference, from degradation products.…”

Section: Resultsmentioning

confidence: 99%

“…Therefore, there was a need for validated methods for the analysis of MT in fish feed as well as in aquatic water systems. An FDA (USA) approved simple specific and robust validated high performance liquid chromatographic (HPLC) method for the determination of MT in fish feed has been published (Marwah et al, 2005). The present work was undertaken to develop a validated liquid chromatography-mass spectrometry (LC-MS) method for the assay of MT in Aquatic water systems.…”

Section: Introductionmentioning

confidence: 99%

Development and validation of a High performance liquid chromatography- Mass spectrometry method for 17a-methyltestosterone in Aquatic water systems

Marwah

Nianzu

Marwah³

et al. 2010

JANS

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17α-Methyltestosterone is used as feed additive to manipulate the gender of fish for aquaculture. Earlier a simple, yet specific and robust validated high performance liquid chromatographic method has been developed for the determination of 17α-methyltestosterone in fish feed. The present work describes a highly sensitive and robust Liquid Chromatography-Mass Spectrometry method for the quantitation of 17α-methyltestosterone in aquatic water systems using 17β-hydroxy-3β-methoxyandrost-5-en-7-one as internal standard. The method was validated in the concentration range of 0.2 to 25 ng of 17α-methyltestosterone on column leading to a limit of quantitation of 0.08 ppb or 0.08 mg/L in water, and has potential to increase the limit of detection and quantitation by an order of magnitude, if required.

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“…Feed samples (FS) and animal feeding water have been proposed as alternative matrixes to control steroids in some countries [4]. Animal feed is a complex matrix very rich in oils and fat, enriched with vitamins, minerals, and preservatives [5]. Moreover, it is not easy to extract the drugs because of the large amounts of proteins and carbohydrates [6].…”

Section: Introductionmentioning

confidence: 99%

Sample preparation for the determination of steroids (corticoids and anabolics) in feed using LC

Muñiz‐Valencia

Ceballos‐Magaña

Gonzalo-Lumbreras

et al. 2008

J of Separation Science

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An improved sample preparation procedure for the determination of 17 steroids (corticoids (CC) and androgenic anabolic steroids (AAS)), used potentially as growth promoters, in feed samples has been developed. This procedure is based on two reported LC-UV methods. The improved procedure includes a leaching process using ACN, saponification, and SPE using polymeric cartridges. The proposed method was validated according to the EU criteria established for quantitative screening methods in PFS. The extraction efficiencies, decision limits (CCalpha) and detection capabilities (CCbeta), for these compounds were in the ranges of 82-100%, 19-40, and 24-53 microg/kg, respectively. The repeatability and the within-laboratory reproducibility at 1.0, 1.5, and 2.0 CCbeta levels were smaller than 10%. Accuracy was in the 97-101% range. The robustness was evaluated using the Youden robustness test. This method was applied to the analysis of steroids in different kinds of FS with satisfactory results.

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Development and validation of a high performance liquid chromatography assay for 17α-methyltestosterone in fish feed

Cited by 23 publications

References 14 publications

Transformation of 17a-methyltestosterone in aquatic-sediment systems

Transformation of 17a-methyltestosterone in aquatic-sediment systems

Development and validation of a High performance liquid chromatography- Mass spectrometry method for 17a-methyltestosterone in Aquatic water systems

Sample preparation for the determination of steroids (corticoids and anabolics) in feed using LC

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