液質(zhì)聯(lián)用法檢測大鼠血漿中纈沙坦的濃度
發(fā)布時(shí)間:2018-03-24 00:40
本文選題:纈沙坦 切入點(diǎn):氯沙坦 出處:《中國臨床藥理學(xué)雜志》2016年10期
【摘要】:目的建立檢測大鼠血漿中纈沙坦?jié)舛鹊囊嘿|(zhì)聯(lián)用方法。方法選擇氯沙坦作為內(nèi)標(biāo),用乙腈沉淀蛋白法處理樣本。色譜柱:Agilent ZORBAX XDBC18(2.1 mm×50 mm,5μm),流動(dòng)相:乙腈-0.1%甲酸水溶液,梯度洗脫,流速:0.3 m L·min~(-1),進(jìn)樣量:1μL,分析時(shí)間:5 min。用電噴霧離子源,多反應(yīng)監(jiān)測模式進(jìn)行正離子檢測?疾煸摲椒ǖ膶傩、標(biāo)準(zhǔn)曲線和定量下限、精密度與回收率、基質(zhì)效應(yīng)、穩(wěn)定性。結(jié)果纈沙坦在10~2000 ng·m L~(-1)內(nèi)線性關(guān)系良好(r=0.999 0),定量下限為10 ng·m L~(-1)。血樣日內(nèi)及日間RSD分別為1.83%~3.83%和5.60%~8.89%,回收率為78.82%~85.98%。室溫放置24h、處理后放置72 h、凍融3次及-20℃凍存1個(gè)月后樣本均保持穩(wěn)定。結(jié)論本方法是一種簡單、快速、靈敏的檢測大鼠血漿中纈沙坦?jié)舛鹊姆椒?可滿足動(dòng)物實(shí)驗(yàn)中低劑量給藥的濃度測定要求。
[Abstract]:Objective to establish a HPLC method for the determination of valsartan in rat plasma. Methods Losartan was selected as internal standard and the sample was treated with acetonitrile precipitation protein method. The mobile phase consisted of acetonitrile-0.1% formic acid solution and gradient elution. The velocity of flow is 0.3 mL / L, the injection amount is 1 渭 L, and the analysis time is 1: 5 min. The positive ion is detected by electrospray ion source and multi-reaction monitoring mode. The specificity, standard curve and quantification limit, precision and recovery rate, matrix effect of the method are investigated. Results the linear relationship of valsartan was good in 10 ~ 2 000 ng / L ~ (-1). The lower limit of quantification was 10 ng / m ~ (L ~ (-1)). The RSD of blood samples was 1.83% and 5.60% respectively. The recovery rate was 78.822 ~ 85.98. At room temperature for 24 h, after treatment for 72 h, freezing and thawing for 3 times and freezing at -20 鈩,
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