Tam Y K, Axelson J E
J Pharm Sci. 1978 Aug;67(8):1073-7. doi: 10.1002/jps.2600670813.
A highly sensitive and specific electron-capture GLC assay capable of detecting picogram quantities of metoclopramide, a procaine derivative, in biological fluids was developed. This assay consisted of extracting metoclopramide from an alkalinized aqueous layer into benzene. A portion of the organic phase was derivatized with heptafluorobutyric anhydride. Quantitative estimation of the derivative was accomplished by adding diazepam, the internal standard, in bezene (750 ng/ml). A calibration curve was prepared for the plasma extracts. Linearity was observed in the range studied (91-825 ng/ml). No interference from endogenous substances was observed. The minimum detectable amount was 1 pg/injection. The structure of the derivative was confirmed by electron-impact and chemical-ionization mass spectrometry. The applicability of this method was shown by a preliminary study of the elimination kinetics of metoclopramide in rats after a 10-mg/kg iv dose.
已开发出一种高灵敏度和特异性的电子捕获气相色谱法，可检测生物体液中皮克量的普鲁卡因衍生物甲氧氯普胺。该方法包括将甲氧氯普胺从碱化水层中萃取到苯中。一部分有机相用七氟丁酸酐进行衍生化。通过在苯（750 ng/ml）中加入内标地西泮来完成衍生物的定量测定。为血浆提取物绘制校准曲线。在所研究的范围内（91 - 825 ng/ml）观察到线性关系。未观察到内源性物质的干扰。最低检测量为1 pg/进样。通过电子轰击和化学电离质谱法确认了衍生物的结构。对10 mg/kg静脉注射剂量后大鼠体内甲氧氯普胺的消除动力学进行的初步研究表明了该方法的适用性。
