Jabor Valquiria Aparecida Polisel, dos Santos Michel David, Bonato Pierina Sueli, Gouvea Dayana Rubio, Lopes Norberto Peporine
University of São Paulo, Faculty of Pharmaceutical Sciences of Ribeirão Preto, Ribeirão Preto, SP, Brazil.
Anal Chim Acta. 2007 Oct 10;601(2):212-7. doi: 10.1016/j.aca.2007.08.034. Epub 2007 Aug 25.
A simple, rapid and sensitive high-performance liquid chromatography method was developed for the analysis of the sesquiterpene lactone 15-deoxygoyazensolide (LAC15-D) in rat plasma samples. The chromatographic separation was achieved on a LiChrospher RP18 column using methanol:water (50:50, v/v) containing 0.6% acetic acid as mobile phase, at a flow rate of 0.7 mL min(-1). UV detection was carried out at 270 nm. Phenytoin was used as internal standard. Prior to the analysis, the rat plasma samples were submitted to liquid-liquid extraction with dichloromethane. The mean absolute recoveries were 73% with R.S.D. values lower than 3.5. The method was linear over the 6.0-2000 ng mL(-1) concentration range and the quantification limit was 6.0 ng mL(-1). Within-day and between-day assay precision and accuracy were studied at three concentration levels (15, 300 and 480 ng mL(-1)) and were lower than 15%. The validated method was used to measure the plasmatic concentration of LAC15-D in rats that received a single intraperitoneal dose of 30 mg kg(-1).
建立了一种简单、快速且灵敏的高效液相色谱法,用于分析大鼠血浆样品中的倍半萜内酯15-脱氧戈亚森内酯(LAC15-D)。色谱分离在LiChrospher RP18柱上进行,以含0.6%乙酸的甲醇:水(50:50,v/v)为流动相,流速为0.7 mL min(-1)。在270 nm处进行紫外检测。苯妥英用作内标。分析前,大鼠血浆样品用二氯甲烷进行液-液萃取。平均绝对回收率为73%,相对标准偏差值低于3.5%。该方法在6.0 - 2000 ng mL(-1)浓度范围内呈线性,定量限为6.0 ng mL(-1)。在三个浓度水平(15、300和480 ng mL(-1))下研究了日内和日间测定的精密度和准确度,均低于15%。经验证的方法用于测定接受30 mg kg(-1)单次腹腔注射的大鼠血浆中LAC15-D的浓度。