Blake J W, Tobin T
Br J Sports Med. 1976 Oct;10(3):129-32. doi: 10.1136/bjsm.10.3.129.
Three gas-liquid chromatographic (G.L.C.) procedures discussed have been designed around the four "esses" of detection tests--speed, sensitivity, simplicity, and specificity. These techniques are admirably applicable to the very low plasma drug levels encountered in blood testing under pre-race conditions. The methods are equally applicable to post-race testing procedures, where both blood and urine samples are tested. Drugs can only rarely be detected by the electron capture detector (E.C.D.) without a prior derivatization step, which conveys to the drug(s) high electron affinity. Because of broad applicability, two derivatizing agents, heptafluorobutyric (HFBA) and pentafluorpropionic (PFPA) anhydrides are employed. The three techniques, allowing broad coverage of various drug classes are: 1) direct derivatization of drugs to form strongly electron capturing amides and esters. 2) reductive fragmentation of drugs with lithium aluminum hydride to form alcohols, with conversion to ester derivatives. 3) oxidative fragmentation of drugs with potassium dichromate to form derivatizable groups, followed by direct derivatization.
所讨论的三种气相色谱(G.L.C.)方法是围绕检测试验的四个“要素”——速度、灵敏度、简便性和特异性设计的。这些技术非常适用于赛前条件下血液检测中遇到的极低血浆药物水平。这些方法同样适用于赛后检测程序,即对血液和尿液样本都进行检测。如果没有事先的衍生化步骤,电子捕获检测器(E.C.D.)很少能检测到药物,衍生化步骤会赋予药物高电子亲和力。由于适用性广泛,使用了两种衍生化试剂,即七氟丁酸(HFBA)和五氟丙酸(PFPA)酐。这三种技术能够广泛覆盖各类药物,它们分别是:1)药物的直接衍生化,以形成强电子捕获酰胺和酯。2)用氢化铝锂对药物进行还原裂解以形成醇类,再转化为酯衍生物。3)用重铬酸钾对药物进行氧化裂解以形成可衍生化基团,然后进行直接衍生化。