Liquid chromatographic purification and detection of anabolic compounds

Ginkel, L. A. van; Jansen, Eugène; Stephany, R. W.; Zoontjes, P.W.; Schwillens, P.L.W.J.; Rossum, H.J. van; Visser, Taco D.

doi:10.1016/0021-9673(92)85690-u

Cited by 23 publications

(11 citation statements)

References 20 publications

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“…Temperature and duration of the enzymatic clevage of conjugated mycotoxins (glucuronides and/or sulfates) were chosen based on a method described by van Ginkel et al [13]. For the SPE sample clean-up a method previously developed in our group was applied [20,21 ].…”

Section: Sample Preparationmentioning

confidence: 99%

“…In contrast, ELISA and RIA offer high sensitivity [11], but, due to cross-reactivities, differentiation between the analytes is not possible and unambiguous analyte identification has to be performed by complementary methods. GC in combination with mass spectrometry (GC-MS) has been frequently used in this field, including for the simultaneous determination of all 5 analytes plus zearelanone (ZAN) [12][13][14], which was reported to be a possible metabolite due to oxidation [ 15]. However, analytical confirmation of these findings is to be regarded as controversial, since results generated via HPLC-DAD measurements could not be supported by parallel GC-MS experiments [ 16].…”

Section: Introductionmentioning

confidence: 98%

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Determination of zeranol, taleranol, zearalenone, α- and β-zearalenol in urine and tissue by high-performance liquid chromatography-tandem mass spectrometry

2000

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Key WordsColumn liquid chromatography Tandem mass spectrometry Zeranol, zearalenone and zearalenol SummaryAn LC-MS/MS method has been developed for the sensitive determination of the anabolic compound zeranol, its epimer taleranol and the mycotoxins zearalenone, azearalenol and fl-zearalenol in animal urine and meat samples. Sample preparation included extraction of meat samples and enzymatic digest of urine samples followed by solid phase extraction with RP-18 columns for sample clean-up. Mass spectrometric determination was carried out with an atmospheric pressure chemical ionisation interface (APCI) in the multi-reaction monitoring mode (MRM). Using the negative ion mode, a limit of detection between 0.1 and 0.5 ppb and a limit of determination between 0.5 and 1 ppb could be achieved. With zearalanone (ZAN) as internal standard, a linear range between 0.5 (1.0) and 100ppb in urine samples (cow, pig) and between 1 and 100 ppb in meat samples (cow, calf, pig) could be established. Depending on the biological matrix and analyte, standard deviations were below 8.5 %, with average recovery rates around 86 % to 102 % in spiked samples. The usefulness of the method developed was demonstrated via several contaminated cow and pig urine samples. the mycotoxins zearalenone (ZON) and e-zearalenol (7-ZOL) that can be carried over from contaminated feedstuffto animals [2][3][4]. ZON, e-ZOL and its epimer/%zearalenol (fl-ZOL) are produced by several Fusarium species that colonize grains [5]. High amounts can be found on maize, wheat, barley and oats. All three compounds exhibit distinct HC

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Section: Sample Preparationmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 98%

Determination of zeranol, taleranol, zearalenone, α- and β-zearalenol in urine and tissue by high-performance liquid chromatography-tandem mass spectrometry

2000

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“…Using HPLC-FLD Dänicke et al investigated the kinetics and metabolism of ZON in young female pigs [12]. In spite of its inherent disadvantages GC coupled with MS has also been applied in this area [13][14][15] but the combination of high selectivity and sensitivity make HPLC-MS and HPLC-MS-MS the most suitable techniques for this task. Jodlbauer et al developed an analysis method to measure ZON, ␣-ZOL, ␤-ZOL, ␣-ZAL and ␤-ZAL simultaneously in urine and bovine or porcine tissue using HPLC-MS-MS after one step solid-phase extraction clean-up [6].…”

Section: Introductionmentioning

confidence: 99%

Determination of zearalenone and its metabolites in urine, plasma and faeces of horses by HPLC–APCI–MS

Songsermsakul

Sontag

Cichna‐Markl

et al. 2006

Journal of Chromatography B

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“…The review of Delaunay-Bertoncini and Hennion [26] gave numerous examples of the application of this approach in pharmaceutical and biomedical fields and emphasized the on-line coupling with chromatographic and electrophoretic separation techniques and other new developments, especially with regards to the future analytical microsystems. The advantages of coupling immunoextraction to HPLC have been investigated by extensive studies for the determination of anabolic steroids in urine [27][28][29].…”

Section: Introductionmentioning

confidence: 99%

Simultaneous determination of nandrolone, testosterone, and methyltestosterone by multi‐immunoaffinity column and capillary electrophoresis

Zhang

2008

Electrophoresis

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A multitarget antibody immunoaffinity column was proposed for the purification and enrichment of nandrolone, testosterone, and methyltestosterone from urine. Nandrolone-3-site substituted antigen was designed and synthesized and the polyclonal antibody was prepared with immunizing rabbits. The stationary phase of the immunoaffinity column was synthesized by covalently bonding the antibodies specific to nandrolone, testosterone, and methyltestosterone onto CNBr-actived Sepharose 4B. The analytes of interest were extracted with a methanol/water mixture in one step. The immunoaffinity column showed high affinity and high selectivity to a class of structurally related compounds. The elution was then transferred to a micellar electrokinetic CE system with a running buffer of sodium borate and sodium cholate for separation and determination. Recoveries of the three steroids from complex matrix were 88-94% with RSD values less than 5.2%. Optimization of the immunoaffinity column purification was achieved and the feasibility of the technique for the analysis of steroid hormone was discussed. The results indicated that the combination of multi-immunoaffinity column and CE was an effective technique, which was rapid, simple, and sensitive for the assay of steroids.

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Liquid chromatographic purification and detection of anabolic compounds

Cited by 23 publications

References 20 publications

Determination of zeranol, taleranol, zearalenone, α- and β-zearalenol in urine and tissue by high-performance liquid chromatography-tandem mass spectrometry

Determination of zeranol, taleranol, zearalenone, α- and β-zearalenol in urine and tissue by high-performance liquid chromatography-tandem mass spectrometry

Determination of zearalenone and its metabolites in urine, plasma and faeces of horses by HPLC–APCI–MS

Simultaneous determination of nandrolone, testosterone, and methyltestosterone by multi‐immunoaffinity column and capillary electrophoresis

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