哌嗪雌酚酮的含量测定方法研究  

Study on the Determination of Piperazinylethylestrone

作　　者：钱广生[1] 韩海[2] 李章万[1] 翁玲玲[3] 郑虎[3] 

机构地区：[1]四川大学华西药学院药物分析教研室,成都610041 [2]暨南大学药学院药物分析教研室 [3]四川大学华西药学院药物化学教研室

出　　处：《四川大学学报（医学版）》2004年第5期711-714,共4页Journal of Sichuan University(Medical Sciences)

基　　金：国家自然科学基金重点项目 (批准号 3 943 0 12 0 )资助

摘　　要：目的　采用非水滴定法和 HPL C- U V法测定哌嗪雌酚酮原料药含量 ,建立柱切换柱前衍生化荧光检测的 HPL C法测定狗血浆中哌嗪雌酚酮含量。方法　分别采用无水冰醋酸为溶剂 ,0 .1mol/ L高氯酸为滴定液 ,结晶紫指示液指示终点的非水滴定法和 HPL C- U V法测定哌嗪雌酚酮原料药含量 ;以 FMOC- CL为衍生化试剂 ,采用柱切换柱前衍生化荧光检测的 HPL C法测定狗血浆中哌嗪雌酚酮含量。结果　非水滴定法日内精密度 (RSD)及日间精密度 (RSD)分别为 0 .2 8%、0 .2 1% ;HPL C- UV法中哌嗪雌酚酮在 1.0 0 1～ 5 .0 0 5μg范围内呈良好的线性关系和重现性 ,方法的检测限为 4 ng(S/ N =3) ;柱切换柱前衍生化荧光检测的 HPL C法中线性范围为 8.4～ 4 2 0 ng/m L ,净化回收率为 77.2 4 %～ 83.10 % ,方法回收率为 98.33%～ 10 3.3% ,日内精密度 (RSD)及日间精密度 (RSD)分别小于 7.7%和 7.3% ,方法的检测限为 1ng(S/ N=3)。结论　以上三种方法简便、准确、重现性好 。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 μg 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. Conclusion 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.

关 键 词：高效液相色谱法 非水滴定法 哌嗪雌酚酮 衍生化 柱切换 

分 类 号：R927[医药卫生—药学]