Delbeke F T, Debackere M
Vakgroep Farmacologie en Toxicologie, Faculteit Diergeneeskunde, Universiteit Gent, Belgium.
J Pharm Biomed Anal. 1993 Apr-May;11(4-5):339-43. doi: 10.1016/0731-7085(93)80026-w.
A method is described for the GC-NPD determination of urinary codeine and morphine after derivatization with trifluoroacetic anhydride. The lower limit for accurate quantitative determination was 0.05 microgram ml-1. After the oral administration of Bisolvon Griblettes corresponding to 30 mg codeine phosphate to seven subjects maximum codeine concentrations were obtained after 1-2 h and codeine remained detectable generally 24 h post dosing. The mean maximum level was 5.1 +/- 2.8 micrograms ml-1 found after enzymatic hydrolysis with Suc Helix pomatia juice (SHP). Based on these and previous results (mean 6.3 +/- 3.4 micrograms ml-1) a threshold level for codeine of 16 micrograms ml-1 is proposed. Significant differences were noticed between urinary codeine concentrations found after enzymatic hydrolysis with SHP, beta-glucuronidase from Patella vulgata and acid hydrolysis, respectively. Generally, highest values were obtained after SHP, while beta-glucuronidase and especially acid hydrolysis resulted in much lower levels. No morphine could be detected after acid hydrolysis. Concerning doping analysis, in particular the uniformity of methods and interpretation of the results, it is recommended that the hydrolysis method should be specified in the rules of those sporting federations allowing codeine and/or morphine.
描述了一种用三氟乙酸酐衍生化后，通过气相色谱-氮磷检测器（GC-NPD）测定尿中可待因和吗啡的方法。准确定量测定的下限为0.05微克/毫升。给7名受试者口服相当于30毫克磷酸可待因的必嗽平胶丸后，1-2小时后可获得可待因的最大浓度，给药后24小时内一般仍可检测到可待因。用蜗牛酶（SHP）进行酶水解后，平均最大浓度为5.1±2.8微克/毫升。基于这些及先前的结果（平均6.3±3.4微克/毫升），提出可待因的阈值水平为16微克/毫升。分别用SHP、紫贻贝β-葡萄糖醛酸酶和酸水解后测定的尿中可待因浓度之间存在显著差异。一般来说，SHP水解后得到的值最高，而β-葡萄糖醛酸酶尤其是酸水解得到的值要低得多。酸水解后未检测到吗啡。关于兴奋剂检测分析，特别是方法的一致性和结果的解释，建议在允许使用可待因和/或吗啡的体育联合会规则中明确水解方法。
