Rapid and sensitive determination of nalmefene in human plasma by gas chromatography-mass spectrometry.
A rapid gas chromatography-mass spectrometric method for the determination of nalmefene in human plasma is described. The procedure involves protein precipitation, extraction with ethanol-chloroform mixture and derivatization with pentafluropropionic anhydride. The deuterated analog of nalmefene, 6beta-naltrexol-d(7), was used as the internal standard. Quantitation was achieved on a HP-1 column (12 mx0.2 mm I.D.) with negative chemical ionization (NCI) using methane:ammonia (95:5) as the reagent gas. The standard curves were fitted using a quadratic equation with the curve encompassing a range of 0.5 to 200 ng/ml, and the intra- and inter-assay variations for three different nalmefene levels were less than 10% throughout. The limit of quantitation was found to be 0.5 ng/ml. The method described is highly specific and reproducible, and could also be applied for the determination of naltrexone and 6beta-naltrexol. Application of the method to actual human plasma samples is demonstrated.
Xie
Shan
S
Analytical Psychopharmacology Laboratory, Nathan Kline Institute, 140 Old Orangeburg Road, Orangeburg, NY 10962, USA. xies@nki.rfmh.org
Suckow
Raymond F
RF
Mason
Barbara J
BJ
Allen
David
D
Cooper
Thomas B
TB
D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D009271:Naltrexone / Q000031:analogs & derivatives* / Q000097:blood*; D009292:Narcotic Antagonists / Q000097:blood*; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
D009292:Narcotic Antagonists; D009271:Naltrexone; C038981:nalmefene