反相高效液相色谱法测定复方盐酸阿米洛利片的有关物质

Determination of Related Substances in Compound Amiloride Hydrochloride Tablets by RP-HPLC

目的建立复方盐酸阿米洛利片中4-氨基-6-氯-1,3-苯基二硫酰胺的测定方法。方法采用十八烷基硅烷键合硅胶柱(250mm×4.6mm,5mm);流动相为磷酸盐缓冲液(取磷酸二氢钾13.6g,加水80mL溶解后,加磷酸调节pH值至3.0,再加水至100mL)-甲醇-水(4∶25∶71);流速:1.0mL·min-1;紫外检测波长为265nm。结果 4-氨基-6-氯-1,3-苯基二硫酰胺与两主要成分盐酸阿米洛利及氢氯噻嗪均良好分离,4-氨基-6-氯-1,3-苯基二硫酰胺在1.0～14.6μg·mL-1范围内与峰面积呈良好线性(r=1.000),最低检测量为2ng。结论该方法能有效地控制复方盐酸阿米洛利片中主要有关物质4-氨基-6-氯-1,3-苯基二硫酰胺,更好地控制药品质量。

Objective To establish a method for determination of 4-amino-6-choloro-1,3-benzenedisulfonamide in compound amiloride hydrochloride tablets. Methods A column packed with octadecylsiance bonded silica gel （ 250 mm × 4. 6 mm,5 μm） was used with the mobile phase of phosphate buffer （ 13. 6 g of monopotassium phosphate being dissolved in 80 mL of water,adjusted with phosphoric acid to a pH of 3. 0,and then with water to 100 mL）-methanol-water（ 4∶ 25∶ 71） . The flow rate was 1. 0 mL·min-1 and the detection wavelength was 262 nm. Results 4-amino-6-choloro-1,3-benzenedisulfonamide and the two main contents of hydrochlorothiazide and amiloride hydrochloride were well separated. A good linear relationship was obtained in the range of 1. 0 ～ 14. 6 μg·mL-1 （ r = 1. 000） . The limit detection was 2 ng. Conclusion This method can effectively control the related substances of 4-amino-6-choloro-1,3-benzenedisulfonamide in compound amiloride hydrochloride tablets and well control the quality of the drug.