新型氨基烷基吡啶抗惊厥药2-(4-氯苯基)氨基-2-(4-吡啶基)乙烷的高效液相色谱分析
High performance liquid chromatographic analysis of a novel aminoalkylpyridine anticonvulsant 2-(4-chlorophenyl)amino-2-(4-pyridyl)ethane.
作者信息
Lin G, Nnane I P, Damani L A, Tse K K, Chow A H, Kadaba P K
机构信息
Department of Pharmacology, The Chinese University of Hong Kong, Shatin, NT.
出版信息
J Pharm Biomed Anal. 1998 Nov;18(3):403-9. doi: 10.1016/s0731-7085(98)00097-1.
A simple, rapid and specific high performance liquid chromatographic (HPLC) method for the quantitation of 2-(4-chlorophenyl)amino-2-(4-pyridyl)ethane (AAP-Cl) and identification of its putative metabolite, 2-(4-chlorophenyl)amino-2-(4-pyridyl)ethanol (beta-AA) in rat blood and urine has been developed. AAP-Cl, beta-AA and an appropriate internal standard were extracted from rat biofluids by a solid phase extraction technique using C18 cartridges prior to the HPLC analysis. The extractibility was 92% for AAP-Cl and 98% for beta-AA. The HPLC analysis employed a symmetrical or standard reversed-phase HPLC column (Apex ODS, 5 microm, 25 cm x 0.46 cm) for blood or urine analysis, a mobile phase of water methanol acetonitrile (40:30:30) containing 20 microl 100 ml(-1) diethylamine at a flow rate of 1 ml min(-1), and UV detection at 254 nm. The limit of detection was 100 ng ml(-1) for both analytes in both blood and urine. The calibration curves for AAP-Cl in rat biofluids were shown to be linear in both low and high concentration ranges (blood: 0-1 and 1-10 microg ml(-1); urine: 0-10 and 10-100 microg ml(-1)) with intra- and inter-day coefficients of variation of no more than 18% for blood and 14% for urine. The method developed was successfully applied to a preliminary analysis of intact AAP-Cl in both blood and urine obtained from rats dosed with AAP-Cl.
已开发出一种简单、快速且特异的高效液相色谱（HPLC）方法，用于定量大鼠血液和尿液中的2 -（4 - 氯苯基）氨基 - 2 -（4 - 吡啶基）乙烷（AAP - Cl），并鉴定其假定代谢物2 -（4 - 氯苯基）氨基 - 2 -（4 - 吡啶基）乙醇（β - AA）。在进行HPLC分析之前，使用C18柱通过固相萃取技术从大鼠生物流体中提取AAP - Cl、β - AA和合适的内标物。AAP - Cl的提取率为92%，β - AA的提取率为98%。HPLC分析采用对称或标准反相HPLC柱（Apex ODS，5μm，25 cm×0.46 cm）进行血液或尿液分析，流动相为含有20μl 100 ml⁻¹二乙胺的水 - 甲醇 - 乙腈（40:30:30），流速为1 ml min⁻¹，在254 nm处进行紫外检测。血液和尿液中两种分析物的检测限均为100 ng ml⁻¹。大鼠生物流体中AAP - Cl的校准曲线在低浓度和高浓度范围内均呈线性（血液：0 - 1和1 - 10μg ml⁻¹；尿液：0 - 10和10 - 100μg ml⁻¹），血液的日内和日间变异系数不超过18%，尿液的不超过14%。所开发的方法成功应用于对给予AAP - Cl的大鼠的血液和尿液中完整AAP - Cl的初步分析。
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