Ludden T M, Lalka D, Wyman M G, Goldreyer B N, Haegele K D, Brooks D T, Davila I, Wallace J E
J Pharm Sci. 1978 Mar;67(3):371-3. doi: 10.1002/jps.2600670326.
An electron-capture GLC method to measure procainamide (0.1-1 microgram/sample) in human serum was developed. An internal standard, p-amino-N-[2-(dipropylamino)ethyl]benzamide, is added to the serum before the sample is alkalinized with pH 10.5 phosphate buffer and extracted with ethyl acetate. The ethyl acetate phase is evaporated to dryness, and the residue is reacted with pentafluoropropionic anhydride. N-Pentafluoropropionyl derivatives of the drug and the internal standard had retention times of 5 and 8 min, respectively, when chromatographed at 235 degrees on a 1-m (4-mm i.d.) glass column packed with 5% OV-17 (carrier gas flow of 40 ml/min). The coefficient of variation was less than 5% for spiked standards. Furthermore, N-acetylprocainamide added to samples did not interfere. One hundred and eighty-six samples from 16 patients receiving procainamide intravenously were assayed by this GLC procedure and by a standard colorimetric method. Linear regression analysis yielded a correlation coefficient of 0.985 (slope, 1.040; intercept, 0.015).
建立了一种电子捕获气相色谱法，用于测定人血清中的普鲁卡因胺（0.1 - 1微克/样品）。在样品用pH 10.5的磷酸盐缓冲液碱化并用乙酸乙酯萃取之前，向血清中加入内标对氨基 - N - [2 - （二丙氨基）乙基]苯甲酰胺。乙酸乙酯相蒸发至干，残余物与五氟丙酸酐反应。当在填充有5% OV - 17的1米（内径4毫米）玻璃柱上于235℃进行色谱分析（载气流速40毫升/分钟）时，药物和内标的N - 五氟丙酰衍生物的保留时间分别为5分钟和8分钟。加标标准品的变异系数小于5%。此外，添加到样品中的N - 乙酰普鲁卡因胺不产生干扰。采用这种气相色谱法和标准比色法对16例静脉注射普鲁卡因胺患者的186份样品进行了检测。线性回归分析得出相关系数为0.985（斜率为1.040；截距为0.015）。
