Analysis of loxoprofen in tablets, patches, and equine urine as tert-butyldimethylsilyl derivative by gas chromatography-mass spectrometry

作者：Kim Youngbae; Seo Chan; Oh Suin; Kwak Juhwan; Jung Sumin; Sin Eunsu; Kim Hyunbin; Ji Moongi; Lee Hyeon Seong; Park Hyung Jin; Lee Gwang; Yu Jundong; Kim Minsoo; Lee Wonjae^*; Paik Man Jeong^*

来源：Archives of Pharmacal Research, 2018, 41(4): 459-466.

DOI：10.1007/s12272-018-1023-5

• Loxoprofen
• tert-Butyldimethylsilyl derivative
• Gas chromatography-mass spectrometry
• Tablet
• Patch
• Equine urine

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.

• 出版日期2018-4