摘要
为建立高效液相色谱法测定氟维司群原料药中有关物质的方法,采用Waters Symmetry C8(150 mm×4.6 mm,3.5µm)色谱柱,以水-乙腈-甲醇(41∶32∶27)为流动相A,以水-乙腈-甲醇(10∶49∶41)为流动相B,流速为2.0 mL·min-1进行梯度洗脱,柱温为40℃;检测波长为225 nm;样品温度为8℃;进样体积为10µL.结果表明:系统适应性试验氟维司群主峰和杂质A的分离度为3.03,大于1.5的标准要求;供试品溶液分别经强酸、强碱、高温、氧化、强光等条件破坏,主峰的纯度角均小于纯度阈值,主峰与相邻峰之间的最小分离度均大于1.5、杂质质量守恒均在在95%～105%之间;已知杂质B、C、D、F定量限分别为4.080、1.940、1.355、1.160µg·mL-1,小于报告阈值0.05%对应的样品浓度;所测单个未知杂质质量分数和总杂质量分数在小于0.1%的情况,重复性和中间精密度RSD分别为9.84%和12.49%;供试品在48h内稳定.
Abstract
A method for the quantitative determination of fulvestrant by HPLC was established.The HPLC method was performed on Waters SunFire Symmetry C8 column(150 mm×4.6 mm,3.5µm).The mobile phase consisted of a mixture of water-acetonitrile-methanol(41∶32∶27)as mobile phase A,and a mixture of water-acetonitrile-methanol(10∶49∶41)as mobile phase B.Gradient elution was used at a flow rate of 2.0 mL·min-1.The wavelength was set at 225 nm.The column temperature was 40℃,the sample temperature was 8℃and the sample size was 10µL.The results indicate that the separation degree between the main peak and im-purity A in the system adaptability test is 3.03,which is greater than the standard requirement of 1.5.The pu-rity angles of the main peak are all below the purity threshold,the minimum separation degree between the main peak and adjacent peaks is greater than 1.5,and the mass conservation of impurities is between 95%and 105%,after the test sample solution is destroyed under conditions such as strong acid,strong alkali,high tem-perature,oxidation,and strong light.The quantitative limit for impurities B,C,D,and F is 4.080,1.940,1.355,1.160 µg·mL-1 respectively,less than the sample concentration corresponding to the reporting threshold of 0.05%.The repeatability and intermediate precision RSDs are 9.84%and 12.49%,when the individual un-known impurity content and total impurity content are less than 0.1%.The test sample solution was found to be stable for up to 48 hours.
基金项目
福建省教育厅2023年度中青年教师教育科研项目(JAT231274)
莆田市科技计划项目(2023SM01)
NETL
NSTL
万方数据