[Study on the determination of piperazinylethylestrone].
OBJECTIVE
To establish an HPLC method and a non-aqueous titration for the determination of piperazinylethylestrone drug substance, and an HPLC method for the determination of piperazinylethylestrone in dog plasma.


METHODS
Anhydrous acetic acid as solvent, 0.1 mol/L perchloric acid as titrant, crystal violet solution as indicator to establish non-aqueous titrations and ODS column as stationary phase, methanol and a mixture of 0. 025 mol/L sodium phosphate monobasic and 0.02 mol/L sodium dedecyl sulfate (80:20) [adjusted with phosphoric acid to a pH (4.8 +/- 0.1)] as mobile phase, 220 nm as detective wavelength to establish HPLC-UV method for determination of piperazinylethylestrone drug substance; FMOC-CL as a derivatization reagent, FD as a detector to establish an HPLC method with derivatization and column switching for determination of piperazinylethylestrone in dog plasma.


RESULTS
The RSD of non-aqueous titrations within-day and between-day were 0.28% and 0.21%, respectively; the established HPLC-UV method had good linearity and precision within the range of 1.001-5.005 microg of piperazinylethylestrone, the detection limit was 4 ng (S/N=3); the linearity of HPLC method with derivatization and column switching was within the range of 8.4-420 ng/ml, the detection limit was 1 ng (S/N=3). The clean-up recoveries were from 77.24% to 83.10%, and the method recoveries were 98.33%-103.3%. The RSD of within-day and between-day were less than 7.7% and 7.3%, respectively.


CONCLUSIONS
The above three methods are simple, accurate and precise for the determination of piperazinylethylestrone drug substance and for the determination of piperazinylethylestrone in dog plasma.
West China School of Pharmacy, Sichuan University, Chengdu 610041, China.
Guang-sheng
GS
Qian
Hai
H
Han
Zhang-wan
ZW
Li
Ling-ling
LL
Weng
Hu
H
Zheng
D000818:Animals; D002851:Chromatography, High Pressure Liquid; D004285:Dogs; D004970:Estrone / Q000031:analogs & derivatives* / Q000032:analysis* / Q000097:blood / Q000737:chemistry
C483802:piperazinyl estrone; D004970:Estrone