10.22376/ijpbs.2019.10.1.p1-12 Volume 4 Issue 3 2013 (July - September) In the present work we have developed a new method for the determination of some Antineoplastic agents i.e. capecitabine, cytarabine, etoposide, doxorubicin hydrochloride and methotrexate in pure form and in their pharmaceutical preparations like xabine (Tab.), xeloda (Tab.), cytabine (Inj.), cytaraside (Vial), etosid (Tab.), peltasol (Inj.), zodox (Vial), oncodox (Inj.), biotrexate (Inj.), and imutrex (Inj.) by using N-chlorosuccinimide (NCS) reagent in acidic medium. This reagent in acidic medium produces chloronium ion (Cl lessThan sup greaterThan + lessThan /sup greaterThan ) which is highly reactive. It may react with allylic hydrogen or hydroxyl group of the substances and forming respective oxidation products. Aliquots containing 1-5 mg of sample were taken in 100 mL erlenmeyer flask followed by the addition of 5mL of 0.02N N-chlorosuccinimide reagent (NCS) and 5mL of 4N hydrochloric acid. The reaction mixture was shaken thoroughly and allowed to react at room temperature (25-30 lessThan sup greaterThan 0 lessThan /sup greaterThan C) for required reaction time (10min.). After the reaction was over 5mL of 5% KI solution was added to it, contents shaken thoroughly and allowed to stand for a minute. The liberated iodine was titrated against 0.02N sodiumthiosulphate solution using starch indicator. A blank experiment was also run under identical conditions using all the reagents except sample. Results were calculated by the difference in the titre value of 0.02N sodiumthiosulphate for blank and actual experiment. Maximum deviation was found within the error of ± 1%. The value of standard deviation (SD), relative standard deviation (RSD) and recovery experiments prove to be precise and reproducible. I.C.SHUKLA, SANJAI KUMAR AND O.P.YADAV Antineoplastic agents, titrimetric method, standard deviation (SD), relative standard deviation (RSD), recovery experiment 55-61