Comparative Study on the Content Determination of Primaquine Phosphate by HPLC and Titration / 中国药房

ABSTRACT

OBJECTIVE:To provide reference for revising the standards of primaquine phosphate in International Pharmacopoe-ia (the fifth edition). METHODS:Based on inspection standards for primaquine phosphate and its preparations in different coun-tries,HPLC,perchloric acid potentiometric titration and sodium nitrite dead-stop titration were adopted to determine and compare the contents of primaquine phosphate. RESULTS:In HPLC,the linear range of primaquine phosphate was 128.1-384.2 μg/ml(r=0.999 9);the limit of detection was 0.18 μg/ml,the limit of quantification was 0.59 μg/ml;RSDs of precision,stability and repro-ducibility tests were lower than 1%;recovery was 99.42%-101.14%(RSD=0.6,n=9);destructive test and durability test showed good specificity;the contents of 3 batches of samples were 92.1%,92.3% and 92.0%,respectively. In perchloric acid potentiomet-ric titration,RSDs of precision and reproducibility tests were 1.6%;the titration jump was not obvious;the contents were 99.1%, 99.7% and 98.7%,respectively. In sodium nitrite dead-stop titration,RSDs of precision and reproducibility tests were lower than 1%;the titration jump was obvious;the contents were 96.9%,97.1% and 96.7%,respectively. Sodium nitrite external indicator ti-tration showed better precision than dead-stop titration;the contents were 99.6%,100.0% and 99.5%,respectively. CONCLU-SIONSPerchloric acid potertiometric titration is simple and rapid,but with relatively poor precision and reproducibility,and it contains quinocide. Sodium nitrite dead-stop titration is simple with good precision and reproducibility but long reaction time,and it also contains quinocide,the HPLC method shows good separation and high accuracy,can effectively separate the quinocide in primaquine phosphate,and it is suitable for the quality control of primaquine phosphate.