【摘要】：目的建立硫酸依替米星原料藥含量測(cè)定和有關(guān)物質(zhì)檢查用的反相高效液相色譜-脈沖安培電化學(xué)(LC-PED)方法。方法以15 m L·L-1三氟乙酸溶液(含500μL·L-1五氟丙酸,1.5 g·L-1無(wú)水硫酸鈉,8 m L·L-150%氫氧化鈉溶液,用50%Na OH調(diào)節(jié)p H值至3.5)-乙腈(96∶4)為流動(dòng)相,流速1.0 m L·min-1,脈沖安培電化學(xué)檢測(cè)器檢測(cè),四波形檢測(cè)電位,柱溫35℃,檢測(cè)器溫度35℃,柱后加0.8 mol·L-1Na OH溶液,流速0.4 m L·min-1。結(jié)果 22個(gè)雜質(zhì)得到分離,可將2010年版《中國(guó)藥典》方法中無(wú)法分離的部分雜質(zhì)有效分離;依替米星在0.24~45μg·m L-1內(nèi)線性關(guān)系良好(r=0.999 7);方法的LOD(S/N=3)為2 ng,LOQ(S/N=10)為6 ng;進(jìn)樣精密度RSD(n=6)為0.8%,含量測(cè)定的重復(fù)性RSD(n=6)為0.7%,中間精密度RSD(n=18)為0.98%;有關(guān)物質(zhì)的雜質(zhì)總量重復(fù)性的RSD(n=6)為1.72%,雜質(zhì)總量中間精密度RSD(n=18)為1.71%;溶液在12 h內(nèi)穩(wěn)定。結(jié)論該方法專屬性好,線性范圍寬,靈敏度高,重復(fù)性優(yōu),已經(jīng)被2015年版《中國(guó)藥典》收載。
[Abstract]:Aim to establish a reversed-phase high performance liquid chromatography-pulse amperometric electrochemical (LC-PED) method for the determination of the content of etimicin sulfate and the determination of related substances. Methods 15 mL 路L-1 trifluoroacetic acid (500 渭 L 路L-1 pentafluoropropionic acid, 1.5 g 路L-1 anhydrous sodium sulfate, 8 mL 路L-150% sodium hydroxide) was used. The mobile phase was adjusted by 50%Na OH to 3.5)-acetonitrile (96:4), the flow rate was 1.0ml 路min-1, the detection potential was detected by pulse amperometric electrochemical detector, the detection potential was four-wave shape, the column temperature was 35 鈩，

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