盐酸非那吡啶有关物质及含量检测方法的改进.docVIP

盐酸非那吡啶盐酸非那吡啶henomenex Luna C18 (2) 柱 (4.6 mm × 250 mm，5 μm) ，以磷酸盐缓冲液（取磷酸氢二铵2.64 g，加水900 m溶解后，用磷酸调节pH值至3.0，加水使成1000 m）- 甲醇（50：50）流检测波长240 nm柱温35 ℃盐酸非那吡啶2,6-二氨基吡啶盐酸非那吡啶0.504 ～ 25.2202,6-二氨基吡啶0.213 ～ 5.3150.103 ～ 2.572盐酸非那吡啶盐酸非那吡啶(Shandong Institute for Food and Drug Control , Jinan 250101) Abstract Objective：To improve the determination method for the contents and related substances of phenazopyridine hydrochloride. Method：HPLC was conducted on a Phenomenex Luna C18 (2)46 mm × 250 mm，5 μm) column with phosphate 李晓燕，女，副主任药师，研究方向：药品分析与检验；TelE-mail：xiaoyanli_l@163﹒com buffer(dissolve 2.64 g of dibasic ammonium phosphate in about 900 mL of water, adjust with phosphoric acid to pH 3.0, dilute with water to 1000 mL)-methanol (50:50) as mobile phase,the flow rate was 1.0 mL﹒min-1 , detected with UV 240 nm and the column temperature of 35℃.Results：An excellent separation was achieved for phenazopyridine hydrochloride, 2,6-diaminopyridine and aniline. The linear range was 0.504 - 25.220μg﹒m L-1 (r =1.0000)and the detection limit was 1.0 ng for phenazopyridine hydrochloride ; The linear range was 0.213 - 5.315μg﹒m L-1 (r = 1.0000)and the detection limit was 0.2 ng for 2,6-diaminopyridine;The linear range was 0.103 - 2.572μg﹒m L-1 (r = 0.9999)and the detection limit was 1.9ng for aniline. Conclusion：The improved method can be used effectively to control the quality of phenazopyridine hydrochloride. Key words: phenazopyridine hydrochloride; related substance; content; HPLC; quality control 盐酸非那吡啶尿路止痛国内有2家企业生产，执行标准为国家食品药品监督管理局标准YBYB收载该对两个现行标准进行比较，两标准均采用HPLC法C18柱检有关物质，但流动相组分、检测波长、色谱图时间及杂质限度规定各不相同。参照USP3版盐酸非那吡啶Agilent1200高效液相色谱仪岛津UV2550紫外分光光度计盐酸非那吡啶对照品中国食品药品检定研究院批号100780-200801，含量99.9%；26-二氨基吡啶上海晶纯试剂有限公司，批号16676，含量98%）；苯胺天津市科密欧化学试剂有限公司含量99.5%盐酸非那吡啶120201，120401，120601）；甲醇为色谱纯磷酸氢二胺、庚烷磺酸钠、三羟甲基基甲烷为分析纯纯化水。色谱柱henomenex Luna C18(2) ( 4.6 mm×250 mm，5μm流动相磷酸盐缓冲液（取磷酸氢二铵2.64 g，加水900 m溶解后，用磷酸调节pH值至3.0，加水使成1000 m）-甲醇（50︰50）；流1.0mL﹒min-1；检测波长240 nm柱温35 ℃；