用于同时定量测定罂粟胶囊中吗啡和可待因的薄层色谱-紫外光密度法和气相色谱-质谱检测法

TLC-UV densitometric and GC-MSD methods for simultaneous quantification of morphine and codeine in poppy capsules.

作者信息

Popa D S, Oprean R, Curea E, Preda N

机构信息

Faculty of Pharmacy, U.M.F. Iuliu Hatieganu, Cluj-Napoca, Romania.

出版信息

J Pharm Biomed Anal. 1998 Dec;18(4-5):645-50. doi: 10.1016/s0731-7085(98)00286-6.

DOI:10.1016/s0731-7085(98)00286-6

PMID:9919965

Abstract

Thin-layer chromatographic (TLC)-UV densitometric and gas-chromatographic-mass spectrometric detection (GC-MSD) methods were developed for simultaneous quantification of morphine and codeine in poppy capsules (Papaver somniferum). Morphine and codeine were isolated by extraction with chloroform: isopropanol (3:1, v/v) at pH = 8.5 and by solid-phase extraction on Snap-Cap cartridges at pH = 8.5. The TLC-UV densitometric quantification was performed by external standard method on silica gel plates using ethyl acetate: toluene: methanol: ammonia (68:17:10:5, v/v) as developing solvent and UV detection at 275 nm. For the GC-MSD analysis, the drugs were derivatized with acetic anhydride: pyridine (1:1, v/v) and separated on a 30 m HP5 capillary column. The quantification was performed using nalorphine as internal standard.

摘要

开发了薄层色谱（TLC）-紫外光密度法和气相色谱-质谱检测（GC-MSD）方法，用于同时定量测定罂粟胶囊（罂粟）中的吗啡和可待因。吗啡和可待因通过在pH = 8.5时用氯仿：异丙醇（3:1，v/v）萃取以及在pH = 8.5时在Snap-Cap柱上进行固相萃取来分离。TLC-紫外光密度法定量采用外标法，在硅胶板上以乙酸乙酯：甲苯：甲醇：氨水（68:17:10:5，v/v）作为展开溶剂，并在275 nm处进行紫外检测。对于GC-MSD分析，药物用乙酸酐：吡啶（1:1，v/v）衍生化，并在30 m HP5毛细管柱上分离。使用烯丙吗啡作为内标进行定量。