Multi-detection of corticosteroids in sports doping and veterinary control using high-resolution liquid chromatography/time-of-flight mass spectrometry

Touber, Manja E.; Engelen, M.C. van; Georgakopoulus, C.; Rhijn, J.A. van; Nielen, Michel W. F.

doi:10.1016/j.aca.2006.09.058

Cited by 85 publications

(41 citation statements)

References 24 publications

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“…LC-MS methods for CC and anabolic steroids in horse urine [19] have also been developed. A LC-TOF-MS method for CC in human and animal urine has also been reported [20]. Although, LC-MS technique is sensitive and can give reliable results, it requires high operating cost and is not available in all laboratories.…”

Section: Introductionmentioning

confidence: 97%

Method development validation for corticoids in animal feed samples by liquid chromatography using a monolithic column

Muñiz‐Valencia

Gonzalo-Lumbreras

Santos-Montes

et al. 2007

J of Separation Science

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A LC method for corticosteroids (CC) determination in poultry feed using a Chromolith column and UV detection has been developed and validated. The method development involved the optimization of different hydro-organic mobile phases using methanol or ACN as organic modifiers, flow rate, and temperature. The optimum separation was achieved at 40 degrees C using ACN/water (21:79 v/v) as mobile phase and 3 mL/min flow rate, allowing the separation to baseline of four out of seven CC in about 10 min. Prior to LC, a sample preparation procedure previously assayed for anabolics was used. It includes a leaching process, saponification of the esters from fatty acids, and SPE. Method validation was carried out according to the EU criteria established for quantitative screening methods. The extraction efficiencies, decision limits (CCalpha), and detection capabilities (CCbeta) for these compounds were in the ranges of 86-92%, 27-36 microg/kg, and 33-43 microg/kg, respectively. The repeatability and the within-laboratory reproducibility at 1, 1.5, and 2 CCbeta concentration levels were smaller than 9.0, 5.0, and 4.2% and 9.4, 6.4, and 4.9%, respectively. The CV values of the robustness test were less than 3.8% and the accuracy was in the range of 98-103%. The proposed method was applied to other feed with satisfactory results.

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Section: Introductionmentioning

confidence: 97%

Method development validation for corticoids in animal feed samples by liquid chromatography using a monolithic column

Muñiz‐Valencia

Gonzalo-Lumbreras

Santos-Montes

et al. 2007

J of Separation Science

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“…Four mass spectrometry analyzers that have been introduced as potential workhorses for this type of analysis are magnetic sector [6,8], Fourier transform ion cyclotron resonance (FTMS) [7,11], quadrupole time-of-flight (Q-TOF) [4,9,12,13], and time-of-flight (TOF) [14,15] mass analyzers. More recently, the Orbitrap [16,17] has been demonstrated to perform exceptionally well as an accurate mass instrument.…”

mentioning

confidence: 99%

“…On the other hand, quadrupole TOF instruments are more readily available, less expensive, and easily coupled with chromatography, but of slightly lower mass accuracy as well (only 25% of measurements Յ1 ppm in one study) [10,20]. Finally, TOF instruments are the most widely available, least expensive, and easily coupled with chromatography, but suffer from the lowest published mass accuracy, usually at or about Ϯ5 ppm [16] with an inter-laboratory comparison showing that 24% of measurements on TOF instruments yielding Ն10 ppm mass accuracy [10]. Further, automation of accurate mass analyses using ESI-TOFMS has been difficult due to dead time effects on the time-to-digital conversion (TDC) circuitry that results in peak shifts to lower masses at high sample concentrations [15,21].…”

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confidence: 99%

Automated sub-ppm mass accuracy on an ESI-TOF for use with drug discovery compound libraries

Stroh¹,

Petucci²,

Brecker³

et al. 2007

J. Am. Soc. Mass Spectrom.

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An automated, routine method to obtain sub-ppm accurate mass data on a benchtop electrospray ionization time-of-flight (ESI-TOF) mass spectrometer is described. Standards in the mass range 114 to 734 Da were analyzed over a 5-day period to demonstrate intra-and interday precision and mean mass accuracy less than 1 ppm. One hundred drug discovery pharmaceutical compounds were used to demonstrate an absolute average mass accuracy of 0.47 Ϯ 0.31 ppm. This is in contrast to previous reports of accurate mass analysis using time-of-flight mass spectrometry (TOFMS) technology that operates within 3 to 5 ppm. The same 100 samples were also analyzed using Fourier transform mass spectrometry (FTMS) technology and yielded comparable results to the TOFMS analysis. (J Am Soc Mass Spectrom 2007, 18, 1612-1616

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“…This technique is especially recommended because of its high resolution and excellent retention time repeatability [15]. Benefits of the UHPLC approach have been experimentally highlighted using fast duty cycle mass analysers such as triple quadrupole or timeof-flight (TOF) mass spectrometers in the anti-doping field [16].…”

Section: Introductionmentioning

confidence: 99%

Approach to chemometrics models by artificial neural network for structure: first applications for estimation retention time of doping agent

Shahpar¹,

Esmaeilpoor

2017

Chem. Method.

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A quantitative structure-retention relationship (QSRR), was developed by using the genetic algorithm-partial least square (GA-PLS), Kernel partial least square (GA-KPLS) and LevenbergMarquardt artificial neural network (L-M ANN) approach for the prediction of the retention time (RT) of the doping agents in urine. The values of the retention time were obtained by using ultra-high-pressure liquid chromatography-quadrupole time-offlight mass spectrometry (UHPLC-QTOF-MS). A suitable set of the molecular descriptors was calculated and the important descriptors were selected by the aid of the GA-PLS and GA-KPLS. By comparing the results, GA-KPLS descriptors are selected for L-M ANN. Finally a model with a low prediction error and a good correlation coefficient was obtained by L-M ANN. This model was used to predict the RT values of some of doping agents which were not used in the modeling procedure. This is the first research on the QSRR of doping agents against the RT using the GA-PLS, GA-KPLS and L-M ANN model. KEYWORDS Graphical AbstractApproach to Chemometrics Models … P a g e | 106

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Multi-detection of corticosteroids in sports doping and veterinary control using high-resolution liquid chromatography/time-of-flight mass spectrometry

Cited by 85 publications

References 24 publications

Method development validation for corticoids in animal feed samples by liquid chromatography using a monolithic column

Method development validation for corticoids in animal feed samples by liquid chromatography using a monolithic column

Automated sub-ppm mass accuracy on an ESI-TOF for use with drug discovery compound libraries

Approach to chemometrics models by artificial neural network for structure: first applications for estimation retention time of doping agent

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