Related substances determination of fulvestrant by HPLC
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.
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