Abu-Qare A W, Abou-Donia M B
Department of Pharmacology and Cancer Biology, Duke University Medical Center, Durham, NC 27710, USA.
Biomed Chromatogr. 2001 Nov;15(7):464-70. doi: 10.1002/bmc.97.
A method was validated and applied for the analysis of the insect growth regulator methoprene [Isopropyl (2E,4E)-11-methoxy-3,7,11-trimethyldodeca-2,4-dienoate], its metabolite methoprene acid, the insecticide permethrin [3-(2,2-dichloro-ethenyl)-2,2-dimethylcyclopropanecarboxylic acid(3-phenoxyphenyl)methylester], and two of its metabolites, m-phenoxybenzyl alcohol and m-phenoxybenzoic acid, in rat plasma and urine using solid-phase extraction and reversed-phase high performance liquid chromatography. The analytes were separated using gradient of 55-100% acetonitrile in water (pH 4.0) at a flow rate ranging between 0.6 and 1.0 mL/min over a period of 20 min, and UV detection at 210 and 254 nm. The retention times ranged from 7.3 to 18.4 min. The limits of detection ranged between 50 and 100 ng/ml, while limits of quantitation were 100-150 ng/mL. Average percentage recovery of five spiked plasma samples was 83.6 +/- 3.9, 80.1 +/- 5.4, 82.1 +/- 4.4, 83.7 +/- 3.9 and 83.1 +/- 4.7, and from urine 79.3 +/- 4.3, 82.0 +/- 5.4, 80.7 +/- 4.2, 78.9 +/- 5.7 and 83.9 +/- 4.5 for methoprene, methoprene acid, permethrin, m-phenoxybenzyl alcohol and m-phenoxybenzoic acid, respectively. The method was linear and reproducible over the range of 100-1000 ng/mL. This method was applied to analyze the above chemicals and metabolites following their combined administration in rats.
已验证并应用一种方法,通过固相萃取和反相高效液相色谱法分析大鼠血浆和尿液中的昆虫生长调节剂烯虫酯[异丙基(2E,4E)-11-甲氧基-3,7,11-三甲基十二碳-2,4-二烯酸酯]、其代谢产物烯虫酸、杀虫剂氯菊酯[3-(2,2-二氯乙烯基)-2,2-二甲基环丙烷羧酸(3-苯氧基苯基)甲酯]及其两种代谢产物间苯氧基苄醇和间苯氧基苯甲酸。分析物在20分钟内以0.6至1.0 mL/分钟的流速,通过在水(pH 4.0)中55 - 100%乙腈的梯度进行分离,并在210和254 nm处进行紫外检测。保留时间范围为7.3至18.4分钟。检测限在50至100 ng/ml之间,定量限为100 - 150 ng/mL。五个加标血浆样品中烯虫酯、烯虫酸、氯菊酯、间苯氧基苄醇和间苯氧基苯甲酸的平均回收率分别为83.6 +/- 3.9、80.1 +/- 5.4、82.1 +/- 4.4、83.7 +/- 3.9和83.1 +/- 4.7,尿液中的平均回收率分别为79.3 +/- 4.3、82.0 +/- 5.4、80.7 +/- 4.2、78.9 +/- 5.7和83.9 +/- 4.5。该方法在100 - 1000 ng/mL范围内呈线性且可重现。该方法用于分析大鼠联合给药后上述化学物质及其代谢产物。