Davidson V P, Traiger G J
Department of Pharmacology and Toxicology, University of Kansas, School of Pharmacy, Lawrence 66045-2500.
J Chromatogr. 1991 Jun 14;567(1):213-20. doi: 10.1016/0378-4347(91)80324-6.
p-Methylthiobenzamide (PMTB) is a thiocarbonyl compound exhibiting marked hepatotoxicity and nephrotoxicity. We describe a high-performance liquid chromatographic method for analyzing PMTB and a metabolite, p-methylthiobenzamide-S-oxide (PMTBSO), from rat plasma using a solid-phase extraction technique. In this way, PMTB and PMTBSO can be extracted from 0.5 ml of plasma and separation achieved by an ODS analytical column in as little as 9 min. The mobile phase used was methanol-water (55:45, v/v) and the wavelength for detection was 290 nm. The limits of detection in plasma were 15 ng/ml for PMTB and 33 ng/ml for PMTBSO; the absolute recovery from spiked plasma samples was greater than 84.4% for both compounds and the internal standard. The method was linear throughout the range used with correlation coefficients greater than 0.969. The intra-day accuracy ranged from 1.52 to 15.23% relative error for the PMTB concentration range 151-3025 ng/ml; accuracy of 4.97% or less was obtained for PMTBSO concentrations of 1672-20,068 ng/ml. The intra-day precision (coefficient of variation) of the procedure was found to be no greater than 5.28% for PMTB and 7.9% for PMTBSO. Inter-day accuracy and precision measurements were similar.
对甲硫基苯甲酰胺（PMTB）是一种表现出明显肝毒性和肾毒性的硫羰基化合物。我们描述了一种高效液相色谱法，用于使用固相萃取技术分析大鼠血浆中的PMTB及其代谢物对甲硫基苯甲酰胺 - S - 氧化物（PMTBSO）。通过这种方法，可从0.5 ml血浆中提取PMTB和PMTBSO，并在短短9分钟内通过ODS分析柱实现分离。所用流动相为甲醇 - 水（55:45，v/v），检测波长为290 nm。血浆中的检测限为PMTB 15 ng/ml，PMTBSO 33 ng/ml；两种化合物及内标物在加标血浆样品中的绝对回收率均大于84.4%。该方法在所使用的整个范围内呈线性，相关系数大于0.969。对于151 - 3025 ng/ml的PMTB浓度范围，日内准确度的相对误差为1.52%至15.23%；对于1672 - 20,068 ng/ml的PMTBSO浓度，获得的准确度在4.97%或更低。发现该方法的日内精密度（变异系数）对于PMTB不大于5.28%，对于PMTBSO不大于7.9%。日间准确度和精密度测量结果相似。
