【摘要】：手性藥物具有含量高、療效好、副作用小等優(yōu)點(diǎn),受到醫(yī)生和患者的廣泛青睞。手性固定相高效液相色譜法是目前最成熟的色譜分離技術(shù)方法之一,因其分離效率高、操作簡便而被廣泛應(yīng)用。本文采用手性固定相技術(shù),通過考察色譜柱類型、流動(dòng)相配比、流速和柱溫對(duì)分離效果的影響,開發(fā)了拆分原料藥右旋酮洛芬氨丁三醇、鹽酸阿托莫西汀及中間體N-甲基帕羅西汀中對(duì)映體雜質(zhì)的高效液相色譜分析方法,具體結(jié)果如下:1、開發(fā)了基于DAICEL OJ-RH色譜柱的手性分離右旋酮洛芬氨丁三醇中對(duì)映體雜質(zhì)的高效液相色譜法。結(jié)果表明,最佳的流動(dòng)相為正己烷:異丙醇:乙酸(9:1:0.03),流速為1.0 mL/min,柱溫為30℃。該方法的定量限為0.243μg/mL,在0.243~30.3μg/mL的濃度范圍內(nèi)相關(guān)系數(shù)R~2=1,回收率在92.8~115.7%,RSD為3.6%。2、開發(fā)了基于CHIRALCEL OD-H色譜柱的手性分離鹽酸阿托莫西汀中對(duì)映體雜質(zhì)的高效液相色譜法。結(jié)果表明,最佳的流動(dòng)相為正己烷:異丙醇:二乙胺(85:15:0.2),流速為1.0 mL/min,柱溫為30℃。該方法的定量限為1μg/mL,在0.90~1.5μg/mL的濃度范圍內(nèi)相關(guān)系數(shù)R~2=0.9983,回收率在86.3~112.8%,RSD為0.9%。3、開發(fā)了基于CHIRALPAK AD-H色譜柱的手性分離N-甲基帕羅西汀中對(duì)映體雜質(zhì)的高效液相色譜法。結(jié)果表明,最佳的流動(dòng)相為正己烷:乙醇:水:三氟乙酸(900:105:2:1.95),流速為1.0 mL/min,柱溫為25℃。該方法的定量限為2.5μg/mL,在2.5~38μg/mL的濃度范圍內(nèi)相關(guān)系數(shù)R~2=0.9909,回收率在109.5~115.6%,RSD為0.8%。
[Abstract]:Chiral drugs have the advantages of high content, good curative effect and little side effect, so they are widely favored by doctors and patients. Chiral stationary phase high performance liquid chromatography (HPLC) is one of the most mature chromatographic separation techniques and has been widely used because of its high separation efficiency and simple operation. The chiral stationary phase technique was used to study the effects of chromatographic column type, mobile phase ratio, flow rate and column temperature on the separation effect. Determination of enantiomers in atomoxetine hydrochloride and its intermediate N-methylparoxetine by high performance liquid chromatography. The results are as follows: 1. The chiral separation of enantiomers from dextoprofen amitriol based on DAICEL OJ-RH column has been developed by high performance liquid chromatography (HPLC). The results showed that the best mobile phase was n-hexane: isopropanol: acetic acid (9: 1: 0.03), the flow rate was 1.0 mL/min, and the column temperature was 30 鈩，

本文編號(hào)：2202160