阴离子交换高效液相色谱法测定3-硝基邻苯二甲酸中杂质4-硝基邻苯二甲酸、邻苯二甲酸的含量  

Determination of 4-Nitrophthalic Acid and O-Phthalic Acid in 3-Nitrophthalic Acid by Anion Exchange High Performance Liquid Chromatography

作　　者：姚枝玉 吴秋娟[2] 董静[2] 李薇[2] 张斐[2] 

机构地区：[1]江苏省食品药品监督检验研究院,南京210008 [2]江苏先声药业有限公司,南京210042

出　　处：《药学与临床研究》2015年第1期30-33,共4页Pharmaceutical and Clinical Research

摘　　要：目的 采用阴离子交换高效液相色谱法对3-硝基邻苯二甲酸及其杂质4-硝基邻苯二甲酸、邻苯二甲酸进行色谱分离,并测定杂质4-硝基邻苯二甲酸、邻苯二甲酸的含量.方法：SIELC Primesep D（4.6 mm×50 mm,5 μm）色谱柱;流动相：0.01% H2SO4水溶液-乙腈,梯度洗脱;流速：1.0 mL·min^-1;柱温：30℃;进样量：5 μL;检测波长：222 nm、226 nm、262 nm.采用杂质外标法对3-硝基邻苯二甲酸样品中4-硝基邻苯二甲酸、邻苯二甲酸进行定量.结果：3种物质在0.5 μg·mL^-1~20 μg·mL^-1范围内线性关系良好（r〉0.9995）, 检测限分别为0.03 μg·mL^-1、0.1 μg·mL^-1、0.05 μg·mL^-1.结论：该方法快速简便,灵敏度高,重现性好,可用于两杂质的定量分析.Objective: To establish a method to determine 4-nitrophthalic acid(4-NPA) and O-phthalic acid(O-PA) in 3-nitrophthalic acid(3-NPA) by anion exchange high performance liquid chromatography.Methods: A SIELC Primesep D column(4.6 mm×50 mm, 5 μm) was used. The mobile phase consisted of0.01% H2SO4 solution and acetonitrile with gradient elution. The flow rate was 1.0 m L·min-1with the column temperature at 30 ℃. The injection volume was 5 μL. UV detection wavelength was set at 262 nm,226 nm and 222 nm. The contents of O-PA and 4-NPA in samples were determined quantitatively by an external standard method. Results: The three substances in the scope of 0.5 μg·m L-1~20 μg·m L-1have good linear relations(r>0.9995), the detection limit of 3-NPA, 4-NPA and O-PA separately was 0.03 μg·m L-1, 0.1 μg·m L-1and 0.05 μg·m L-1. Conclusion: The method is simple, accurate and suitable for the determination of 4-NPA and O-PA in 3-NPA.

关 键 词：阴离子交换 3-硝基邻苯二甲酸 4-硝基邻苯二甲酸 邻苯二甲酸 

分 类 号：R927.2[医药卫生—药学]