高效液相色谱法测定米力农原料药中4-吡啶甲酸的含量

Determination of isonicotinic acid in milrinone by HPLC

目的建立米力农原料药中杂质4删：啶甲酸的高效液相测定方法，并和主峰、其他杂质达到有效分离。方法采用高效液相色谱法，选用辛烷基键合硅胶色谱柱，以磷酸氢二钾溶液（取磷酸氢二钾2．7g，加水800mL溶解后，加三乙胺2．4mL，用磷酸调节pH值至7．5）-乙腈（80：20）为流动相，流速为1．0mL·min^-1温为25％，检测波长为220nm。结果异烟酸在0．998～2．994mg·L^-1内线性关系良好（r=0．9999，n=5），平均加样回收率为99．85％，RSD为0．38％（n=9）。结论该方法简便快速，结果准确，可做为4．吡啶甲酸含量的检测方法。

Objective To establish an HPLC method for the determination of isonicotinic acid in milrinone. Methods Liquid chroma tography was used. The column was C8 column. The mobile phase was the mixture of pH 7.5 phosphate buffer（ Dissolving 2.7 g of dibas ic potassium phosphate in 800 mL of water, adding 2.4 mL of triethylamine, adjusting with phosphoric acid to a pH of about 7.5, and mix. ） and acetonitrile （80： 20）. The flow rate was 1.0 mL . min^-1. The column temperature was at 25 ℃. The detection wavelength was 220 nm. Results Isonicotinie acid was linear in the range from 0. 998 to 2.994 mg . L^- 1 （ r = 0.999 9, n = 5 ）. The average recovery was 99.85% ,and RSD was 0.38% （n =9）. Conclusion The method is simple,rapid,and accurate,which can be used as the quality con trol method.