Leis H J, Windischhofer W, Wintersteiger R
Universität Kinderklinik, Department of Mass Spectrometry, Graz, Austria.
Biol Mass Spectrom. 1994 Oct;23(10):637-41. doi: 10.1002/bms.1200231006.
A selected ion monitoring stable isotope dilution gas chromatographic/negative ion chemical ionization mass spectrometric assay for amphetamine in human plasma is described. The preparation of (2H5)amphetamine from the intact target molecule and its use as an internal standard for quantitative gas chromatography/mass spectrometry are demonstrated. Derivatization to the highly electrophoric pentafluorobenzoate with pentafluorobenzoyl chloride in hexane resulted in high yield of prominent negative ions with methane as a moderating gas. The pentafluorobenzoate was also found to be superior to fluoroacyl derivatives with respect to sample handling due to its lower volatility. The method presented permits detection of amphetamine in the low picogram per millilitre range and should thus be highly useful for its trace level determination in forensic, toxicological and pharmaceutical applications.
本文描述了一种用于测定人血浆中苯丙胺的选择离子监测稳定同位素稀释气相色谱/负离子化学电离质谱分析法。展示了从完整的目标分子制备(2H5)苯丙胺及其作为定量气相色谱/质谱内标物的用途。在己烷中用五氟苯甲酰氯将其衍生化为高亲电性的五氟苯甲酸酯,以甲烷作为缓和气体时,可产生高产率的显著负离子。还发现五氟苯甲酸酯由于挥发性较低,在样品处理方面优于氟酰基衍生物。所提出的方法能够检测低至皮克/毫升范围内的苯丙胺,因此对于其在法医、毒理学和制药应用中的痕量水平测定应该非常有用。