首页> 外国专利> METHOD OF DETERMINING 2,6-BISBIS(BETA-HYDROXYETHYL)AMINO-4,8-DI-N-PYPERIDINO-PYRIMIDO(5,4-D)PYRIMIDINE IN BIOLOGICAL MATERIAL

METHOD OF DETERMINING 2,6-BISBIS(BETA-HYDROXYETHYL)AMINO-4,8-DI-N-PYPERIDINO-PYRIMIDO(5,4-D)PYRIMIDINE IN BIOLOGICAL MATERIAL

机译:测定生物材料中2,6-双[双(双(羟乙基)氨基)氨基] -4,8-​​二-吡啶基-嘧啶并(5,4-D)嘧啶的方法

摘要

FIELD: analytical methods in toxicological chemistry.;SUBSTANCE: invention relates to methods for determining title compound in biological material for use in practice of chemicotoxicological and clinical laboratories. Biological tissue is disintegrated, two times infused with acetone each time for 30 min, resulting extracts are combined, combined extracts are filtered, filtrate is evaporated to give dry residue, the latter is dissolved in chloroform and extracted with 0.1 hydrochloric acid, acid extract is washed with diethyl ether, alkalinized with 10% sodium hydroxide solution to pH 8-10, saturated with sodium chloride, and extracted with ethylacetate. Ethylacetate extract is separated, dehydrated, and evaporated to give residue, which is dissolved in mixture acetonitrile/1 N sulfuric acid (8:2 v/v), and chromatographed on column packed with sorbent "Silasorb C-18" having particle size 30 μm while using acetonitrile/1 N sulfuric acid (8:2 v/v) as mobile phase. Fractions of eluate containing subject substance are combined and optical density of combined eluate is measured at wavelength 286 nm.;EFFECT: reduced analysis time, increased degree of recovery, accuracy, and sensitivity of determination.;3 tbl, 2 ex
机译:技术领域本发明涉及确定用于化学毒理学和临床实验室的生物材料中标题化合物的方法。分解生物组织,每次两次注入丙酮30分钟,合并提取液,将合并的提取液过滤,滤液蒸发,得到干燥的残留物,将其溶于氯仿中,然后用0.1盐酸萃取,用乙醚洗涤,用10%氢氧化钠溶液碱化至pH 8-10,用氯化钠饱和,并用乙酸乙酯萃取。分离乙酸乙酯萃取液,脱水并蒸发,得到残余物,将其溶于乙腈/ 1 N硫酸混合物(8:2 v / v)中,并在装有粒径为30的吸附剂“ Silasorb C-18”的色谱柱上进行色谱分离使用乙腈/ 1 N硫酸(8:2 v / v)作为流动相时,其粒径为μm。合并含有目标物质的洗脱液馏分,并在286 nm波长处测量合并的洗脱液的光密度。效果:缩短分析时间,提高回收率,准确性和测定灵敏度; 3 tbl,2 ex

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