Cone E J, Darwin W D
Biomed Mass Spectrom. 1978 Apr;5(4):291. doi: 10.1002/bms.1200050404.
A selected ion recording using chemical ionization (methane) is described for the simultaneous measurement of hydrocodone, hydromorphone and their respective 6alpha- and 6beta-hydroxymetabolites in human urine. The samples were acid-hydrolyzed, extracted and derivatized by silylation. Only partial resolution of the components on 3% OV-17 was achieved but was sufficient for their determination. The [M+1]+ ions of the drugs and metabolites as well as the [M+29]+ ion of the internal standard were recorded. The assay was sensitive down to c. 0.01 microgram ml-1. The relative standard deviation of standards processed along with the samples ranged from 4.5-8.2%. Hydrocodone was found to be metabolized in man primarily by O-demethylation and 6-keto reduction. Hydromorphone was excreted mainly in the unchanged form (after acid-hydrolysis) with only minor amounts of the 6-hydroxymetabolites being detected. A lack of stereoselectivity in the metabolic reduction ofhydrocodone was observed.
本文描述了一种使用化学电离（甲烷）的选择离子记录法，用于同时测定人尿中的氢可酮、氢吗啡酮及其各自的6α-和6β-羟基代谢物。样品经酸水解、萃取并用硅烷化进行衍生化处理。在3% OV - 17上仅实现了部分组分分离，但足以进行测定。记录了药物和代谢物的[M + 1]+离子以及内标的[M + 29]+离子。该测定法的灵敏度低至约0.01微克/毫升。与样品一起处理的标准品的相对标准偏差为4.5 - 8.2%。发现氢可酮在人体内主要通过O - 去甲基化和6 - 酮还原进行代谢。氢吗啡酮主要以未变化的形式（酸水解后）排泄，仅检测到少量的6 - 羟基代谢物。观察到氢可酮代谢还原过程中缺乏立体选择性。
