Hashimoto S, Sakurai E, Mizobuchi M, Takahashi S, Yamamoto K, Momose T
Biomed Mass Spectrom. 1984 Jan;11(1):50-4. doi: 10.1002/bms.1200110110.
The capillary gas chromatographic negative ion chemical ionization mass spectrometric assay of peptidoaminobenzophenone (2-o-chlorobenzoyl-4-chloro-N-methyl-N'-glycylglycinanilide) (1) and its three metabolites in human plasma reported in Part 1 was changed as follows: (1) the reagent gas was changed to ammonia from isobutane; (2) each unlabelled compound (1%) was added to the deuterium-labelled compound used as the internal standard; (3) all samples were injected in the splitless mode; (4) one more metabolite, lormetazepam, was determined; (5) day-to-day reproducibility was checked in the range of 1-50 ng ml-1. Points 1 to 3 improved the preciseness with small-sized samples. Calibration curves were prepared in the range of 0.5-50 ng ml-1. Plasma levels of compound 1 and its four metabolites in 10 volunteers were measured.
第1部分报道的人血浆中肽氨基二苯甲酮(2 - o - 氯苯甲酰基 - 4 - 氯 - N - 甲基 - N'- 甘氨酰甘氨酸苯胺)(1)及其三种代谢物的毛细管气相色谱负离子化学电离质谱分析方法更改如下:(1)反应气由异丁烷改为氨;(2)将每种未标记化合物(1%)添加到用作内标的氘代标记化合物中;(3)所有样品均采用不分流模式进样;(4)测定了另外一种代谢物氯硝西泮;(5)在1 - 50 ng ml-1范围内检查了日间重现性。要点1至3提高了小体积样品的精密度。在0.5 - 50 ng ml-1范围内绘制校准曲线。测定了10名志愿者体内化合物1及其四种代谢物的血浆水平。