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目的:采用同位素比质谱方法对使用某些类固醇制剂(本文选用雄烯二酮)后的尿样中的代谢物进行同位素比值测定,以检测尿中类固醇的来源,区分是自然代谢物还是使用类固醇制剂后的代谢物,并确定使用制剂后用此方法检测到阳性结果的时间。方法:采用酶解、高效液相色谱(HPLC)等方法对尿样中内源性类固醇激素进行酶解游离型、分离,再经气相色谱/燃烧炉/同位素比值质谱方法检测代谢物及内源性类固醇参照物13C与12C同位素含量的相对比值(δ值)。将被检测物与参照物同位素比值的差值与判别标准值比较,进行来源判定,并用正常人尿样进行对照。结果:使用雄烯二酮制剂后尿样中内源性类固醇激素代谢物δ值低于未使用的正常值,提示有外源性类固醇摄入。用同位素比质谱方法可在4或5天之内检测到阳性结果。结论:利用同位素比质谱法可在一定时间内检测尿中类固醇代谢物的来源。
OBJECTIVE: To determine the source of steroid in urine by using isotope ratio mass spectrometry to determine the isotope ratio of metabolites in urine sample after the use of certain steroid preparations (in this paper, androstenedione), whether it is a natural metabolite or a steroid The metabolites after formulation, and to determine the time after using the method to detect positive results. Methods: Enzymolysis, high performance liquid chromatography (HPLC) were used to detect endogenous steroid hormones in urine samples by enzymatic dissociation and separation. The metabolites and endogenous sources were detected by gas chromatography / combustor / isotope ratio mass spectrometry The relative ratio (delta value) of the sex steroid reference 13C and 12C isotope content. The difference between the isotope ratio of the test substance and the reference substance was compared with the discriminant standard value, and the source judgment was made and the urine samples of normal people were used for comparison. Results: The δ value of the endogenous steroid hormone metabolites in urine samples after the use of the androstenedione preparation was lower than the unused normal values, suggesting the exogenous steroid ingestion. Positive results can be detected within 4 or 5 days using isotope ratio mass spectrometry. Conclusion: The source of steroid metabolites in the urine can be detected within a certain period of time using isotope ratio mass spectrometry.