抗心律失常药丙吡胺的分光光度测定新法

New spectrophotometry for determination of antiarrhythmic disopyramide

建立了一种用于抗心律失常药丙吡胺的分光光度测定新法。此法基于下述4个步骤:(1)丙吡胺分子中的氮原子能与过量四苯硼钠(Ph_4B^-Na^+)定量反应生成沉淀;(2)滤液中余量的四苯硼钠(Ph_4B^-Na^+)负一价大阴离子(Ph_4B^-)与Cu^+-2,9-二甲基-1,10-菲罗啉(正一价大阳离子)螯合物生成缔合物;(3)这黄色的缔合物经异戊醇定量地萃取;(4)在最大吸收波长470纳米处相对于参比溶液测定吸光度。在最佳条件下,校正曲线的线性关系良好,线性回归系数R2=0.9991,遵守比尔定律的浓度范围是0~2×10^(-4) mol/L的,丙吡胺。此法用于丙吡胺模拟注射液的测定,其标准加入的回收率范围为99.76%~100.66%,日内和日间变异系数分别是0.25%和0.42%。测定3×10^(-4) mmol的Ph4B-时,■2×10^(-4) mmol量的Na^+,K^+,Ag^+,Mg^(2+),Zn^(2+),Co^(2+),Cd^(2+),Al^(3+)及■5×10^(-5)mmol量的Ca^(2+),Sr^(2+),Ba^(2+),Fe^(2+),Fe^(3+)和■5×10^(-4) mmol量的Cl^-,NO_3^-不干扰。而■5×10^(-5) mmol量的Cu^(2+)能抢夺Cu+-2,9-二甲基-1,10-菲罗啉螯合物中的2,9-二甲基-1,10-菲罗啉,从而有干扰,但加入盐酸羟胺将Cu2+还原成Cu+,即可消除此干扰。本法简便,可靠,未见国内外报道。

It is based on the fellowing four steps： （1）The nitrogen atoms in the disopyramide molecule reacts quantitatively with excessive sodium tetraphenylboron to form precipitate; （2）The residual anion of tetraphenylboron in filtrate forms yellow associate molecule with copperion（I）--2,9--dimethyl phenanthroline chelate in the buffer medium of acetic acid-sodium acetate; （3）The yellow associate moleculeis quantitatively extracted by isoamylol; （4）Then absorbance of the isoamylol extact layer of the yellow associated moleculeis determined in comparision with reference solution at 470 nm.. Under optimum conditions, the coefficient of linear regression is R2 =0. 9991, the Beer＇s law is obeyed in the concentration range of 0--2（ × 10^-4）mol/L of disopyramide. The method is applicated to determinate isopyramide in the simulated inject solution and the recoveries of standard addition are 99.76%- 100.66%. Within- and between-day coefficients of variation are 0.25 % and 0.42 %, respectively. When determing 3 × 10^-4 mmol Ph4 B^- , under the conditions of ≤2×10^-4 mmol of Na^＋ ,K^＋ ,Ag^＋ ,Mg^2＋ ,Zn^2＋ ,Co^2＋ ,Cd^2＋ ,Al^3＋ ,≤5 × 10^-5mmol of Ca^2＋ , Sr^2＋ , Ba^2＋ , Fe^2＋ , Fe^3＋ and 45× 10^-4 mmol of Cl^- , NO^3- does not interference with the results. The method is simple and reliable.