Lombardi F, Crolla T
Analytical Development Laboratory, Zambeletti S.p.A., Milan, Italy.
J Pharm Sci. 1988 Aug;77(8):711-4. doi: 10.1002/jps.2600770814.
A specific, sensitive, accurate, and precise capillary gas chromatographic assay for determining trace levels of hydroxylamine, a well-known mutagen, in propionohydroxamic acid bulk drug and oral preparations is described. The analytical procedure involves derivatization in a nonaqueous medium with cyclohexanone and use of an internal standard. The derivative is then determined by capillary GC with a cool on-column injector and a nitrogen-selective detector. Effects of different matrices on the measurement were also determined. The lower limit of quantitation was 7 ppm, and the response was linear from 10 to 260 ppm. The procedure is simple and rapid enough for routine purposes.
本文描述了一种用于测定丙酸异羟肟酸原料药和口服制剂中痕量羟胺（一种著名的诱变剂）的特异性、灵敏性、准确性和精密性的毛细管气相色谱分析方法。该分析方法包括在非水介质中用环己酮进行衍生化反应并使用内标。然后通过配备冷柱头进样器和氮选择性检测器的毛细管气相色谱法测定衍生物。还测定了不同基质对测量的影响。定量下限为7 ppm，响应在10至260 ppm范围内呈线性。该方法简单快速，适用于常规分析。
