Cámpora Pamela, Bermejo Ana María, Tabernero María Jesús, Fernández Purificación
Institute of Legal Medicine, Forensic Toxicology Service, Faculty of Medicine, University of Santiago de Compostela, Spain.
Rapid Commun Mass Spectrom. 2006;20(8):1288-92. doi: 10.1002/rcm.2449.
An analytical method for the simultaneous determination of codeine, morphine and 6-acetylmorphine (6AM) in human oral fluid was developed. The method involves liquid-liquid extraction in Toxitubes A, derivatization with 99:1 (v/v) N,O-bis(trimethylsilyl)trifluoroacetamide (BSTFA)/trimethylchlorosilane (TMCS), and gas chromatography/mass spectrometry with positive chemical ionization (GC/PCI-MS) determination. The detector response was linear over the concentration range 30-500 ng/mL with coefficients of correlation higher than 0.99. The precision was acceptable with coefficients of variation less than 7.5%. The limits of detection achieved were 0.7 ng/mL for codeine, 2.0 ng/mL for morphine, and 0.6 ng/mL for 6AM. The method proposed was applied to 80 oral fluid samples from opiates users, 98% of which were positive for the three analytes. Human oral fluid is a suitable biological fluid for the determination of opiates by GC/PCI-MS.
建立了一种同时测定人唾液中可待因、吗啡和6-乙酰吗啡(6AM)的分析方法。该方法包括在Toxitubes A中进行液-液萃取,用99:1(v/v)的N,O-双(三甲基硅基)三氟乙酰胺(BSTFA)/三甲基氯硅烷(TMCS)进行衍生化,以及采用正化学电离的气相色谱/质谱联用(GC/PCI-MS)测定。检测器响应在30 - 500 ng/mL浓度范围内呈线性,相关系数高于0.99。精密度可接受,变异系数小于7.5%。可待因的检测限为0.7 ng/mL,吗啡为2.0 ng/mL,6AM为0.6 ng/mL。所提出的方法应用于80份来自阿片类药物使用者的唾液样本,其中98%的样本对这三种分析物呈阳性。人唾液是通过GC/PCI-MS测定阿片类药物的合适生物样本。