Development and validation of a high performance liquid chromatography-tandem mass spectrometry for the determination of etodolac in human plasma.
A simple and specific method using a one-step liquid-liquid extraction (LLE) with butyl acetate followed by high performance liquid chromatography (HPLC) coupled with positive ion electrospray ionization tandem mass spectrometry (ESI-MS/MS) detection was developed for the determination of etodolac in human plasma, using indomethacin as an internal standard (IS). Chromatographic separation was performed isocratically using a Capcellpak MGII C(18) column with 65% acetonitrile and 35% water containing 10mM ammonium formate (adjusted to pH 3.5 with formic acid). Acquisition was performed in multiple reaction monitoring (MRM) mode by monitoring the transitions: m/z 287.99>172.23 for etodolac and m/z 357.92>139.01 for IS. The method was validated to determine its selectivity, linearity, sensitivity, precision, accuracy, recovery and stability. The limit of quantitation (LLOQ) was 0.1microg/mL with a relative standard deviation of less than 15%. The devised method provides an accurate, precise and sensitive tool for determining etodolac levels in plasma.
Lee
Hyun-Soo
HS
College of Pharmacy, Kyung-Hee University, Hoegi-Dong, Dongdaemun-Ku, Seoul 130-701, Republic of Korea.
Kang
Il-Mo
IM
Lee
Heon-Woo
HW
Seo
Ji-Hyung
JH
Ryu
Ju-Hee
JH
Choi
Sang-Jun
SJ
Lee
Myung-Jae
MJ
Jeong
Seo-Young
SY
Cho
Young-Wuk
YW
Lee
Kyung-Tae
KT
D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000097:blood*; D002138:Calibration; D002851:Chromatography, High Pressure Liquid; D017308:Etodolac / Q000097:blood*; D006801:Humans; D007213:Indomethacin / Q000097:blood / Q000493:pharmacokinetics; D011786:Quality Control; D015203:Reproducibility of Results; D053719:Tandem Mass Spectrometry
D000894:Anti-Inflammatory Agents, Non-Steroidal; D017308:Etodolac; D007213:Indomethacin