【摘要】：目的:建立高效液相色譜法測(cè)定安立生坦片中有關(guān)物質(zhì)。方法:采用安捷倫ZORBAX SB-Aq(4.6mm×250 mm,5μm)色譜柱,流動(dòng)相A為5 mmol·L~(-1)磷酸二氫鉀溶液(p H 3.0),流動(dòng)相B為乙腈,以1.0m L·min~(-1)的流速進(jìn)行梯度洗脫,檢測(cè)波長(zhǎng)為210 nm,柱溫25℃,以自身對(duì)照法測(cè)定安立生坦片中有關(guān)物質(zhì)。結(jié)果:安立生坦與各雜質(zhì)及降解產(chǎn)物能夠完全分離(分離度大于2.0);供試品溶液在24 h內(nèi)穩(wěn)定性良好;安立生坦和2-羥基-3-甲氧基-3,3-二苯基丙酸(雜質(zhì)A)、(S)-1-(4-氯苯基)乙胺(雜質(zhì)B)、3,3二苯基-2,3-環(huán)氧丙酸甲酯(雜質(zhì)C)、2-羥基-3-甲氧基-3,3二苯基丙酸甲酯(雜質(zhì)D)、4,6-二甲基-2-甲基-磺酰嘧啶(雜質(zhì)E)和4,6-二甲基-2-(2,2-二苯基-乙烯氧基)嘧啶(雜質(zhì)F)的定量限分別為0.66、0.64、0.65、1.31、0.65、0.63和1.32 ng,相對(duì)校正因子分別為1.00、1.08、2.20、1.09、1.10、2.54和1.07;安立生坦質(zhì)量濃度在0.5~5.0μg·m L~(-1)范圍內(nèi)線性良好(r0.999 9),各雜質(zhì)質(zhì)量濃度在0.125~2.5μg·m L~(-1)范圍內(nèi)線性良好(r0.999),雜質(zhì)加樣回收率(n=9)在95.8%～103.7%之間;重復(fù)性和中間精密度符合規(guī)定。經(jīng)檢測(cè),3批安立生坦片中雜質(zhì)A含量均為0.01%。結(jié)論:經(jīng)驗(yàn)證本方法準(zhǔn)確、靈敏,精密度高,耐用性和專(zhuān)屬性強(qiáng),可用于安立生坦片中有關(guān)物質(zhì)的測(cè)定。
[Abstract]:Objective: to establish a high performance liquid chromatography (HPLC) method for the determination of related substances in Anlishentan tablets. Methods: an Agilent ZORBAX SB-Aq (4.6mm 脳 250mm ~ 5 渭 m) column was used. The mobile phase A was 5 mmol L ~ (-1) potassium dihydrogen phosphate solution (p H 3.0, and the mobile phase B was acetonitrile. Gradient elution was carried out at a flow rate of 1.0 mL 路min ~ (-1). The detection wavelength was 210nm and the column temperature was 25 鈩，

本文編號(hào)：2158777