Libeer J C, Schepens P
J Pharm Sci. 1978 Mar;67(3):419-21. doi: 10.1002/jps.2600670343.
A specific GLC method for the determination of microgram quantities of the central stimulant pemoline in biological fluids is described. Extraction problems due to the low solubility of pemoline are avoided by acid hydrolysis of the drug to 5-phenyl-2,4-oxazolidinedione, which then can be easily isolated by two-phase extraction with dichloromethane, ether, or chloroform. Amide-imide tautomerism enables a cleanup of the extract. Quantitative determination at the microgram level is done on a methylated fraction of the dichloromethane extract by GLC using a suitable internal standard. For supporting evidence of the GLC method's specificity, the compound is also identified by examining an aliquot of the final dichloromethane extract by TLC.
本文描述了一种用于测定生物流体中微克量中枢兴奋剂匹莫林的特定气相色谱法。通过将药物酸水解为5-苯基-2,4-恶唑烷二酮，避免了由于匹莫林溶解度低而导致的萃取问题，然后可以通过用二氯甲烷、乙醚或氯仿进行两相萃取轻松分离。酰胺-酰亚胺互变异构可对提取物进行净化。使用合适的内标，通过气相色谱法对二氯甲烷提取物的甲基化部分进行微克级的定量测定。为了支持气相色谱法特异性的证据，还通过薄层色谱法检查最终二氯甲烷提取物的等分试样来鉴定该化合物。
