Mogi M, Ito T, Matsuki Y, Kurata Y, Nambara T
Hatano Research Institute, Food and Drug Safety Centre, Kanagawa, Japan.
J Chromatogr. 1987 Jul 24;399:234-50.
A method for the determination of isofloxythepin in biological fluids by gas chromatography-mass spectrometry is described. Isofloxythepin was readily converted into the trimethylsilyl ether by treatment with N,O-bis(trimethylsilyl)trifluoroacetamide. This derivative was separated on a 5% OV-101 column and determined, employing newly prepared isofloxythepin-d7 as an internal standard. Clean-up of isofloxythepin in blood and urine was efficiently achieved by back-extraction with hexane or hexane-toluene (9:1) under acidic and basic conditions, while isofloxythepin glucuronide in biological fluids was isolated by ion-exchange chromatography on Dowex 50W-X4 resin. The detection limit of isofloxythepin by this method was 50 pg. The blood and urine levels of isofloxythepin after oral administration of the drug to dogs were monitored by the proposed method.
描述了一种通过气相色谱 - 质谱法测定生物体液中异氟磷的方法。异氟磷通过用N，O - 双（三甲基硅基）三氟乙酰胺处理很容易转化为三甲基硅基醚。该衍生物在5% OV - 101柱上分离，并以新制备的异氟磷 - d7作为内标进行测定。在酸性和碱性条件下，通过用己烷或己烷 - 甲苯（9:1）反萃取有效地实现了血液和尿液中异氟磷的净化，而生物体液中的异氟磷葡萄糖醛酸苷则通过在Dowex 50W - X4树脂上的离子交换色谱法分离。该方法测定异氟磷的检测限为50 pg。通过所提出的方法监测了给狗口服该药物后血液和尿液中异氟磷的水平。
