US EPA

3859251 

Journal Article 

Determination of naloxone and naltrexone as perfluoroalkyl ester derivatives by electron-capture gas-liquid chromatography 

Sams, RA; Malspeis, L 

1976 

1 

Journal of Chromatography
ISSN: 0021-9673 

Elsevier 

125 

2 

409-420 

English 

977685 

10.1016/s0021-9673(00)83372-5 

WOS:A1976CL97800004 

https://linkinghub.elsevier.com/retrieve/pii/S0021967300833725
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An electron-capture gas chromatographic method is described for the determination of naloxone and naltrexone as the perfluoroalkyl esters. Each compound serves as internal standard for determination of the other. The method permits quantitation of 2-100 ng of either compound. Conditions for derivatization with heptafluorobutyric anhydride (HFBA), pentafluoropropionic anhydride (PFPA), and trifluoroacetic anhydride (TFAA) have been investigated. When catalyzed with pyridine, derivatization with HFBA and PFPA at 70 degrees gives naloxone and naltrexone triesters. Evidence for triester formation was obtained from gas chromatography-methane chemical ionization mass spectrometry and infrared spectral analysis. It was found that both the HFB and PFP triesters are suitable for quantitation of the narcotic antagonists, the HFB derivatives having greater stability than the PFP derivatives. The TFA derivatives are substantially less stable. 

Anhydrides; Chromatography, Gas; Chromatography, Liquid; Mass Spectrometry; Naloxone/analogs & derivatives/analysis; Naltrexone/analysis