Optimization of solid-phase extraction for the liquid chromatography-tandem mass spectrometry analysis of basic drugs in equine urine

액체크로마토그래피-텐덤질량분석법을 위한 경주마 소변 중 염기성 약물의 고체상 추출법 최적화

  • Shin, Hyun Du (Racing Laboratory, Korea Racing Authority) ;
  • Yang, Ji Suk (Racing Laboratory, Korea Racing Authority) ;
  • Jung, Mihye (College of Pharmacy, Chung-Ang University) ;
  • Kim, Hyung-Seung (College of Pharmacy, Chung-Ang University) ;
  • Youm, Jeong-Rok (College of Pharmacy, Chung-Ang University) ;
  • Hu, Man Bae (Racing Laboratory, Korea Racing Authority) ;
  • Kim, Sung Jean (Racing Laboratory, Korea Racing Authority) ;
  • Han, Sang Beom (College of Pharmacy, Chung-Ang University)
  • 신현두 (한국마사회 도핑검사소) ;
  • 양지숙 (한국마사회 도핑검사소) ;
  • 정미혜 (중앙대학교 약학대학) ;
  • 김형승 (중앙대학교 약학대학) ;
  • 염정록 (중앙대학교 약학대학) ;
  • 허만배 (한국마사회 도핑검사소) ;
  • 김상진 (한국마사회 도핑검사소) ;
  • 한상범 (중앙대학교 약학대학)
  • Received : 2008.07.09
  • Accepted : 2008.09.09
  • Published : 2008.10.25

Abstract

A procedure based on solid-phase extraction (SPE) followed by liquid chromatography-tandem mass spectrometry has been developed for the simultaneous analysis of 55 basic drugs in equine urine. The test scope covers diversified classes of drugs including some ${\beta}$-blockers, ${\beta}$-agonists, antihypotensives, CNS stimulants, sedatives, tranquilizers, antidepressants, antihypertensives and so on. LC-MS/MS separation and quantification was carried out in positive electrospray ionization and multiple reaction monitoring (MRM) mode. Four different brands of mixed mode cation exchange SPE sorbents; UCT XTRACT$^{(R)}$ XRDAH, Supelco DSC-MCAX$^{(R)}$, Varian Bond Elut Certify$^{(R)}$ and Waters Oasis$^{(R)}$ MCX were compared. The UCT XTRACT$^{(R)}$ XRDAH sorbent provided the best results in the preconcentration of samples, yielding relative recoveries higher than 80% except for terbutaline (41.3%), salbutamol (71.5%), heptaminol (70.7%), phenylpropanolamine (66.3%). Detection limits of the target drugs provided by the proposed analytical procedure were between 0.2~8.3 ng/mL.

Keywords

Basic drugs;Equine urine;SPE;LC-MS/MS

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