本文選題：二維色譜　切入點(diǎn)：甲氨蝶呤　出處：《分析化學(xué)》2015年01期 　論文類型：期刊論文

【摘要】：建立了反向模式-強(qiáng)陽(yáng)離子交換-反向模式(Reversed phase-strong cation exchange-reversed phase)二維色譜平臺(tái)測(cè)定人血漿中甲氨蝶呤濃度的方法。樣品經(jīng)三氯醋酸沉淀蛋白后,在ASTON C8一級(jí)柱(100 mm×4.6 mm,5μm)上完成初分離,通過(guò)六通閥切換,經(jīng)ASTON SCX中間級(jí)(20 mm×4.6 mm,5μm)二次分離和儲(chǔ)存,在SAC C8二級(jí)柱(100 mm×4.6 mm,5μm)上完成最后分離,并測(cè)定。一級(jí)柱流動(dòng)相為10 mmol/L醋酸銨-乙腈(90∶10,V/V,以醋酸調(diào)至p H 3.8),流速為1.0 m L/min;中間級(jí)流動(dòng)相為10 mmol/L H3PO4溶液(p H 3.0);二級(jí)柱流動(dòng)相為50 mmol/L醋酸銨-乙腈(87∶13,V/V,以醋酸調(diào)至p H 5.2),流速為1.2 m L/min,檢測(cè)波長(zhǎng)306 nm。單次分析時(shí)間4 min,線性范圍0.09~5.1μmol/L,檢出限為0.005μmol/L,日內(nèi)RSD小于1.8%,日間RSD小于3.5%,相對(duì)回收率99.1%~101.25%,絕對(duì)回收率85.7%~86.4%。本方法簡(jiǎn)便、準(zhǔn)確,適合日常血藥濃度監(jiān)測(cè)和藥代動(dòng)力學(xué)研究。
[Abstract]:A two-dimensional chromatographic platform for the determination of methotrexate in human plasma by reverse mode, strong cation exchange and reverse mode was established. The sample was precipitated by trichloroacetic acid and separated on a ASTON C8 column of 100mm 脳 4.6mm ~ 5 渭 m. Through the six way valve switch, the final separation was completed on the SAC C8 secondary column (100mm 脳 4.6mm / 5 渭 m) by ASTON SCX intermediate stage 20mm 脳 4.6mm / 5 渭 m) secondary separation and storage, and the final separation was carried out on the SAC C8 second stage column (100mm 脳 4.6mm / 5 渭 m). The mobile phase was 10 mmol/L ammonium acetate-acetonitrile 90: 10 V / V, adjusted to pH 3.8U with acetic acid, the flow rate was 1.0 mL / min, the intermediate mobile phase was 10 mmol/L H _ 3PO _ 4 solution and the second stage column was 50 mmol/L ammonium acetate -acetonitrile 8713 V / V / V, adjusted to acetic acid. The detection wavelength was 306 nm 路min. The linear range was 0.09 渭 mol / L, the detection limit was 0.005 渭 mol / L, the detection limit was 0.005 渭 mol / L, the intra-day RSD was less than 1.8, the relative recovery rate was 99.1g / min, the absolute recovery was 85.7 渭 mol / L, and the absolute recovery was 86.40.The method was simple and convenient. It is accurate and suitable for daily blood concentration monitoring and pharmacokinetic study.
【作者單位】： 中南大學(xué)湘雅醫(yī)院藥學(xué)部;中南大學(xué)藥學(xué)院;
【分類號(hào)】：R96;O657.72

【共引文獻(xiàn)】

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本文編號(hào)：1643198