Thermospray liquid chromatography—mass spectrometry of corticosteroids

Steffenrud, S.; Maylin, G. A.

doi:10.1016/0378-4347(92)80243-j

Cited by 26 publications

(6 citation statements)

References 26 publications

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“…The abuse of these substances has been a constant challenge for anti‐doping agencies, so the control of corticosteroids is absolutely necessary, not only to ensure the existence of clean and drug‐free sports but also to protect the athletes from masked injuries and additional effort caused by the concealing of pain, both in human and in animals. Owing to the recognized side effects of these drugs, it is not surprising that 19 publications about the development of analytical methods specifically to detect corticosteroids in samples from racing horses were found since 1990 11,13,227–243 . In a review of clinical use and characteristics of the corticosteroids, several complications were associated with their chronic abuse in horses, namely, increased rate of joint breakdown, septic arthritis, degenerative joint disease, suppression of the hypothalamic–pituitary adrenal system, increased susceptibility to infection, and laminitis, a painful and potentially crippling disease resulting from the inflammation of the lamina of the hoof 244 …”

Section: Resultsmentioning

confidence: 99%

“…Owing to the recognized side effects of these drugs, it is not surprising that 19 publications about the development of analytical methods specifically to detect corticosteroids in samples from racing horses were found since 1990. 11,13,[227][228][229][230][231][232][233][234][235][236][237][238][239][240][241][242][243] In a review of clinical use and characteristics of the corticosteroids, several complications were associated with their chronic abuse in horses, namely, increased rate of joint breakdown, septic arthritis, degenerative joint disease, suppression of the hypothalamic-pituitary adrenal system, increased susceptibility to infection, and laminitis, a painful and potentially crippling disease resulting from the inflammation of the lamina of the hoof. 244 Cortisol, also known as hydrocortisone, is considered the precursor of all glucocorticoid drugs.…”

Section: Corticosteroidsmentioning

confidence: 99%

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Doping detection in animals: A review of analytical methodologies published from 1990 to 2019

Moreira

Carmo

Pinho

et al. 2021

Drug Testing and Analysis

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Despite the impressive innate physical abilities of horses, camels, greyhounds, or pigeons, doping agents might be administered to these animals to improve their performance. To control these illegal practices, anti‐doping analytical methodologies have been developed. This review compiles the analytical methods that have been published for the detection of prohibited substances administered to animals involved in sports over 30 years. Relevant papers meeting the search criteria that discussed analytical methods aiming to detect and/or quantify doping substances in animal biological matrices published from 1990 to 2019 were considered. A total of 317 studies were included, of which 298 were related to horses, demonstrating significant advances toward the development of doping detection methods for equine sports. However, analytical methods for the detection of doping agents in sports involving other species are lacking. Due to enhanced accuracy and specificity, chromatographic analysis coupled to mass spectrometry detection is preferred over immunoassays. Regarding biological matrices, blood and urine remain the first choice, although alternative biological matrices, such as hair and feces, have been considered. With the increasing number and type of drugs used as doping agents, the analytes addressed in the published papers are diverse. It is very important to continue to detect and quantify these drugs, recognizing those that are most frequently used, in order to punish the abusers, protect animals' health, and ensure a healthier and genuine competition.

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Section: Resultsmentioning

confidence: 99%

Section: Corticosteroidsmentioning

confidence: 99%

Doping detection in animals: A review of analytical methodologies published from 1990 to 2019

Moreira

Carmo

Pinho

et al. 2021

Drug Testing and Analysis

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“…It helped to detect problematic drugs from diuretics (chlorothiazide), stimulants (methyl phenidate, mesocarb) and steroids (3-OH-stanozolol) thereby making one versatile method for various drugs. The ionization and fragmentation pattern differs for each category of drugs; the results suggest that glucocorticosteroids are neutral compounds to ionize[ 9 ] whereas steroids and diuretics are polar[ 10 ] and easily fragmentable. Also observed was no polarity switching between chlorothiazide (detected at a retention time of 2.98 min in negative mode) and methyl phenidate (detected at a retention time of 3.00 min in positive mode) though they are co-eluting substances.…”

Section: Discussionmentioning

confidence: 99%

A simple and rapid ESI-LC-MS/MS method for simultaneous screening of doping agents in urine samples

Reddy¹,

Beotra²,

Jain³

et al. 2009

Indian J Pharmacol

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Objective:The use of performance enhancing substances is banned in sports by the World Anti-Doping Agency (WADA). Though most prohibited substances can be detected by GC/MS, inclusion of corticosteroids and designer drugs has made it essential to detect these critical doping agents on LC/MS/MS due to their better separation and detection.Materials and Methods:A common extraction procedure for the isolation of acidic, basic and neutral drugs from urine samples was developed. A total of 28 doping drugs were analyzed on API 3200 Triple quadrupole mass spectrometer using C18 column in atmospheric pressure electrospray ionization. The mobile phase composition was a mixture of 1% formic acid and acetonitrile with gradient time period.Results:The method developed was very sensitive for detection of 28 doping agents. The linearity was performed for each drug and the total recovery percentage ranged from 57 to 114. Limit of detection is found to be 0.5 ng/ml for carboxy finasteride and 1-5 ng/ml for other drugs. The method was successfully used to detect positive urine samples of 3-OH-stanozolol, methyl phenidate, mesocarb, clomiphene metabolite and carboxy finasteride.Conclusion:The method developed based on controlled pH extraction method and HPLC-mass spectrometry analysis allowed better identification and confirmation of glucocorticosteroids and a few other drugs in different categories. The validated method has been used successfully for testing of 1000 In-competition samples. The method helped in detection of chemically and pharmacologically different banned drugs in urine in a single short run at a minimum required performance limit set by WADA.

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“…Several analytical methods such as LC-MS/MS 3 , HPLC [4][5][6][7][8] , and UV-spectrophotometric 9 methods have been reported for the estimation of acyclovir alone or with other drugs. In same way, many analytical methods like LC-MS/MS [10][11][12] , HPLC 13,14 and HPTLC 15,16 methods were available for the assay of hydrocortisone alone or with other drugs. The literature study did not revealed any reported method for simultaneous HPLC method for assay of acyclovir and hydrocortisone in dosage form.…”

Section: Introductionmentioning

confidence: 98%

Analytical Quality by Design (AQbD) Approach to Liquid Chromatographic Method for Quantification of Acyclovir and Hydrocortisone in dosage forms

Peraman

Kalva²,

Shanka³

et al. 2014

Analytical Chemistry Letters

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Analytical quality by design (AQbD) based high performance liquid chromatographic (HPLC) method for routine analysis of acyclovir and hydrocortisone in dosage form has been developed on C18 column using experimental design. Central composite design (CCD) was adopted in assessment of method responses and robustness. In experimental design, resolution (Y 1 ) and separation factor (Y 2 ) were tested method critical parameters such as pH (X 1 ), % aqueous in mobile phase (X 2 ) and flow rate (X 3 ). Two models for retention time (Y 1 ) and separation factor (Y 2 ) were obtained and then interpreted statistically. Chromatographic optimum range for each input variable (Xn) was obtained through analysis of constructed models and contour plots. The predicted data from response models for resolution time (Y1) and separation factor (Y2) were statistically significant. Then, these variables were used in verification of method performance characteristics such as accuracy and precision within the method operable range for robustness. The robustness behavior of the method was verified at different points and the result was good with more than 40 % of aqueous phase (X2) at pH of 6.0 (X1) at a flow rate of 0.9 ml min -1 (X3). The method has proven and suitable for regulatory flexibility.

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Thermospray liquid chromatography—mass spectrometry of corticosteroids

Cited by 26 publications

References 26 publications

Doping detection in animals: A review of analytical methodologies published from 1990 to 2019

Doping detection in animals: A review of analytical methodologies published from 1990 to 2019

A simple and rapid ESI-LC-MS/MS method for simultaneous screening of doping agents in urine samples

Analytical Quality by Design (AQbD) Approach to Liquid Chromatographic Method for Quantification of Acyclovir and Hydrocortisone in dosage forms

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