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Quantification and validation of nine nonsteroidal anti-inflammatory drugs in equine urine using gas chromatography-mass spectrometry for doping control.
Drug Testing and Analysis ( IF 2.6 ) Pub Date : 2020-06-28 , DOI: 10.1002/dta.2864 Eylem Funda Göktaş 1 , Erol Kabil 1 , Filiz Arıöz 2
Drug Testing and Analysis ( IF 2.6 ) Pub Date : 2020-06-28 , DOI: 10.1002/dta.2864 Eylem Funda Göktaş 1 , Erol Kabil 1 , Filiz Arıöz 2
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Nonsteroidal anti‐inflammatory drugs (NSAIDs) are commonly used in therapeutic doses in human and veterinary medicine for the treatment of inflammation, pain, and fever. A method for the simultaneous determination of nine NSAIDs, known as therapeutic prohibited substances, in equine urine was developed and fully validated according to the European Commission Decision 2002/657/EC and Association of Official Racing Chemists criteria. The validation was performed for naproxen, flunixin, ketoprofen, diclofenac, eltenac, meclofenamic acid, phenylbutazone, vedaprofen, and carprofen in equine urine in accordance with the International Screening Limits (ISL) regulated by International Federation of Horseracing Authorities. After basic hydrolysis, samples were extracted with a C18 cartridge using automated solid‐phase extraction. Several derivatization reagents were investigated, and trimethylphenylammonium hydroxide/methanol (20/80, v/v) was selected. Analyses were carried out using gas chromatography–mass spectrometry with selected ion monitoring mode, but the method can be applied to a large number of analytes. The within‐laboratory reproducibility was not more than 12.8% (≤15%), and mean relative recoveries ranged from 91.1% to 104.1% for inter‐day and intra‐day precision. The decision limits (CCα) and detection capabilities (CCβ) were evaluated at concentrations near the ISL for each therapeutic substance. The validation results demonstrated that the method is highly reproducible, easily applicable, and suitable for the analysis of some NSAIDs in equine urine that have not been previously published. Finally, the method was also applied to known positive samples.
中文翻译：
使用气相色谱-质谱法对马尿中的九种非甾体类抗炎药进行定量和验证，以进行掺杂控制。
非甾体类抗炎药（NSAIDs）通常以人和兽药的治疗剂量用于炎症，疼痛和发烧的治疗。根据欧洲委员会决定2002/657 / EC和官方赛车化学家协会的标准，开发了一种同时测定马尿中9种非甾体类抗炎药的方法，并被确认为有效方法。根据国际赛马联合会规定的国际筛查限量（ISL），对马尿中的萘普生，氟尼辛，酮洛芬，双氯芬酸，eltenac，甲氯芬那酸，苯基丁酮，韦达洛芬和卡洛芬进行了验证。碱性水解后，使用自动固相萃取用C18柱萃取样品。研究了几种衍生试剂，并选择了三甲基苯基氢氧化铵/甲醇（20/80，v / v）。使用气相色谱-质谱联用选定的离子监测模式进行了分析，但该方法可以应用于大量分析物。实验室内的可重复性不超过12.8％（≤15％），日间和日间精度的平均相对回收率在91.1％至104.1％之间。决策限制（抄送 日间和日内精度为1％到104.1％。决策限制（抄送 日间和日内精度为1％到104.1％。决策限制（抄送α）和检测能力（CC β）在ISL对于每个治疗物质邻近浓度进行评价。验证结果表明，该方法具有高度重现性，易于应用且适用于分析马尿中某些尚未公开的NSAID。最后，该方法还应用于已知的阳性样品。
更新日期：2020-06-28
中文翻译：
使用气相色谱-质谱法对马尿中的九种非甾体类抗炎药进行定量和验证，以进行掺杂控制。
非甾体类抗炎药（NSAIDs）通常以人和兽药的治疗剂量用于炎症，疼痛和发烧的治疗。根据欧洲委员会决定2002/657 / EC和官方赛车化学家协会的标准，开发了一种同时测定马尿中9种非甾体类抗炎药的方法，并被确认为有效方法。根据国际赛马联合会规定的国际筛查限量（ISL），对马尿中的萘普生，氟尼辛，酮洛芬，双氯芬酸，eltenac，甲氯芬那酸，苯基丁酮，韦达洛芬和卡洛芬进行了验证。碱性水解后，使用自动固相萃取用C18柱萃取样品。研究了几种衍生试剂，并选择了三甲基苯基氢氧化铵/甲醇（20/80，v / v）。使用气相色谱-质谱联用选定的离子监测模式进行了分析，但该方法可以应用于大量分析物。实验室内的可重复性不超过12.8％（≤15％），日间和日间精度的平均相对回收率在91.1％至104.1％之间。决策限制（抄送 日间和日内精度为1％到104.1％。决策限制（抄送 日间和日内精度为1％到104.1％。决策限制（抄送α）和检测能力（CC β）在ISL对于每个治疗物质邻近浓度进行评价。验证结果表明，该方法具有高度重现性，易于应用且适用于分析马尿中某些尚未公开的NSAID。最后，该方法还应用于已知的阳性样品。
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