Introduction of tamoxifen Pharmacopoeia

Identification (1) Take a proper amount of this product, add 5ml of acetic anhydride-pyridine (1: 5), shake well, and heat in water bath until the color of the solution changes from yellow to red. (2) Take this product, add absolute ethanol to dissolve and dilute it into a solution containing about 65438 00μ g per ml, and determine it by UV-Vis spectrophotometry (Appendix 4A), with maximum absorption at 238nm and 278nm. (3) The infrared absorption spectrum of this product should be consistent with the control spectrum (spectrum group 265); If not, take this product and recrystallize it with acetone for determination. Check loss on drying, take this product, dry it at 105℃ for 4 hours, and the weight loss shall not exceed 0.5% (Appendix VIII L). A new system is used to manipulate substances in the dark. Take this product, weigh it accurately, add mobile phase to dissolve it, dilute it quantitatively, and make a solution containing about 65438 0.5 mg per ml as the test solution; Accurately measure an appropriate amount and dilute it quantitatively with mobile phase to make a solution containing 7.5 micrograms per milliliter as a control solution; Take another E- isomer reference substance, accurately weigh it, add mobile phase to dissolve it, and dilute it quantitatively to make a solution containing about 7.5 micrograms per milliliter as the reference substance solution. According to the experiment of high performance liquid chromatography (Appendix V D), octadecylsilane bonded silica gel was used as filler, phosphate buffer (0.9g sodium dihydrogen phosphate and 4.8g N, N- dimethyl octyl amine were dissolved in water and diluted to 1000ml, and the pH value was adjusted to 3.0 with phosphoric acid)-acetonitrile (60: 40) was used as mobile phase, and the wavelength was detected. Take 10μl control solution and the mixed solution of the control solution, inject it into the liquid chromatograph, and adjust the detection sensitivity, so that the peak height of tamoxifen citrate chromatographic peak is about 30% of the full scale, the theoretical plate number calculated by E- isomer peak is not less than 2000, and the separation degree between E- isomer peak and main component peak (Z- isomer) should be greater than 3.0. Then accurately measure 65438 00μ l of test solution, reference solution and reference solution, and inject them into the liquid chromatograph respectively, and record the chromatogram to twice the retention time of the principal component peak. If there is a peak with the same retention time as the isomer peak in the chromatogram of the test sample, its peak area shall not be greater than the main peak area of the reference solution (0.5%); If there are other impurity peaks, the area of a single impurity peak shall not be greater than the main peak area of the control solution (0.5%), and the sum of other impurity peak areas shall not be greater than twice the main peak area of the control solution (1.0%). Content determination: take about 0.35g of this product, weigh it accurately, add 50ml of glacial acetic acid, dissolve it at low temperature, add crystal violet indicator 1 drop, and titrate the solution with perchloric acid (0. Lmol/L) until the solution turns blue-green, and the titration result is corrected by blank test. Every 1 ml of perchloric acid titration solution (0.lmol/L) is equivalent to 56.36 mg of C26H29No C6H807. Anti-tumor drugs. Store in a cool, sealed and dry place.