Kim S H, Park J M, Ryu C K, Lee M G
College of Pharmacy, Seoul National University, Kwanak-Gu, South Korea.
Res Commun Mol Pathol Pharmacol. 1999 Jan;103(1):101-7.
A high-performance liquid chromatographic method was developed for the determination of a new phospholipase A2 inhibitor, NQ12, in human plasma and urine. The sample preparation was simple: 2 volumes of acetonitrile were added to the biological samples to deproteinize it. A 50-microl aliquot of the supernatant was injected onto a C18 reversed-phase column. The mobile phase employed was 0.05M acetate buffer (pH 3) : acetonitrile : methanol (30:45:25, v/v/v) and run at a flow rate of 1.5 ml/min. The column effluent was monitored by a UV detector set at 298 nm. The retention times for NQ12 and the internal standard were approximately 5.5 and 7.0 min, respectively. The detection limits for NQ12 in human plasma and urine were all 20 ng/ml. The coefficients of variation of the assay (within-day and between-day) were generally low (below 11.8%) for human plasma and urine. No interferences from endogenous substances were found.
建立了一种高效液相色谱法，用于测定人血浆和尿液中一种新型磷脂酶A2抑制剂NQ12。样品制备方法简单：向生物样品中加入2倍体积的乙腈进行蛋白沉淀。取50微升上清液注入C18反相柱。所用流动相为0.05M醋酸盐缓冲液（pH 3）：乙腈：甲醇（30:45:25，v/v/v），流速为1.5毫升/分钟。柱流出物用设定在298纳米的紫外检测器监测。NQ12和内标的保留时间分别约为5.5分钟和7.0分钟。人血浆和尿液中NQ12的检测限均为20纳克/毫升。该测定法（日内和日间）的变异系数对于人血浆和尿液通常较低（低于11.8%）。未发现内源性物质的干扰。
