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KMID : 0043320180410040459
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Archives of Pharmacal Research
2018 Volume.41 No. 4 p.459 ~ p.466
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Analysis of loxoprofen in tablets, patches, and equine urine as tert-butyldimethylsilyl derivative by gas chromatography-mass spectrometry
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Kim Young-Bae
Seo Chan
Oh Su-In
Kwak Ju-Hwan
Jung Su-Min
Sin Eun-Su
Kim Hyun-Bin
Ji Moon-Gi
Lee Hyeon-Seong
Park Hyung-Jin
Lee Gwang
Yu Jun-Dong
Kim Min-Soo
Lee Won-Jae
Paik Man-Jeong
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Abstract
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Loxoprofen is a non-steroidal anti-inflammatory drug of the 2-arylpropionic acid type, which has used to treat musculoskeletal disorders in the horse racing industry. However, it has also used illicitly to mask clinical signs of inflammation and pain in racehorses. Thus, its accurate analysis has become an important issue in horse doping laboratories. In this study, an analytical method of loxoprofen was developed as tert-butyldimethylsilyl (TBDMS) derivative by gas chromatography-mass spectrometry (GC?MS). Characteristic fragment ions of [M-15], [M-57], and [M-139] permitted the accurate and selective detection of loxoprofen. Under optimal conditions, this method showed good linearity (r?≥?0.999) in the range of 10?500 ng/mL, repeatability (% relative standard deviation?=?5.6?8.5), and accuracy (% relative error?=???0.3?0.9) with a detection limit of 1.0 ng. When applied to the analysis of loxoprofen in tablet and patch products, loxoprofen was positively identified as TBDMS derivative by GC?MS. The present method provided rapid and accurate determination of loxoprofen in patch and tablet products. Levels of loxoprofen were highest in equine urine at 0.5 and 1 h after oral administration with single dose (3 mg/kg) to three horses, and then rapidly reduced to below the lower limit of quantification at 24 h. Therefore, the present method will be useful for the pharmacokinetic study and doping tests for loxoprofen and other similar acidic drugs in horses.
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KEYWORD
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Loxoprofen, tert-Butyldimethylsilyl derivative, Gas chromatography-mass spectrometry, Tablet, Patch, Equine urine
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