Johnson E L, Pachla L A
J Pharm Sci. 1984 Jun;73(6):754-6. doi: 10.1002/jps.2600730612.
A sensitive, specific, and rapid high-performance liquid chromatographic procedure was developed for the determination of pirmenol in human biological fluids. Plasma or urine samples were alkalinized and extracted with cyclohexane. The organic extract was evaporated to dryness, reconstituted with the mobile phase, and then chromatographed on a microparticulate spherical trimethylsilane stationary phase with UV detection at 254 nm. The procedure for the assay of pirmenol in plasma was linear from 0.125 to 5.0 micrograms/mL. The reproducibility of the peak area ratios of the standard curves had relative standard deviations between 7.7 and 1.8% and a relative error of 0-4.6% over the linear range. The accuracy for the determination of pirmenol in human plasma containing 0.5, 2.5, and 4.0 micrograms/mL had relative errors of 9.0, 3.8, and 3.6%, respectively. Thirty compounds were tested and found not to interfere in the assay of the drug in plasma, and the method was found to be suitable for clinical samples. The urine procedure was linear between 1.0 and 30.0 micrograms/mL. The reproducibility of the peak areas of the standard curves had relative standard deviations that ranged from 1.9 to 6.2% over the linear range. The accuracy for the determination of pirmenol in human urine containing 5.0, 17.5, and 25.0 micrograms/mL had relative errors of 1.4, 0.5, and 2.8%, respectively.
建立了一种灵敏、特异且快速的高效液相色谱法,用于测定人体生物样品中的吡美诺。将血浆或尿液样品碱化,并用环己烷萃取。有机萃取液蒸发至干,用流动相复溶,然后在微粒球形三甲基硅烷固定相上进行色谱分析,于254nm波长处进行紫外检测。血浆中吡美诺的测定方法在0.125至5.0微克/毫升范围内呈线性。标准曲线峰面积比的重现性在该线性范围内的相对标准偏差为7.7%至1.8%,相对误差为0至4.6%。测定含0.5、2.5和4.0微克/毫升吡美诺的人血浆时,其准确度的相对误差分别为9.0%、3.8%和3.6%。测试了30种化合物,发现它们不干扰血浆中该药物的测定,该方法适用于临床样品。尿液测定方法在1.0至30.0微克/毫升之间呈线性。标准曲线峰面积的重现性在该线性范围内的相对标准偏差为1.9%至6.2%。测定含5.0、17.5和25.0微克/毫升吡美诺的人尿液时,其准确度的相对误差分别为1.4%、0.5%和2.8%。