HPLC测定注射用对氨基水杨酸钠中的有关物质

Determination of the related substances in Sodium aminosalicylate for injection by HPLC

目的采用离子对HPLC法测定注射用对氨基水杨酸钠(PAS-Na)中的有关物质。方法采用十八烷基硅烷键和硅胶为填充剂,流动相为乙腈-10%四丁基氢氧化铵溶液-0.05 mol·L^(-1)NaH_2PO_4(100∶2∶900),流速1.0 mL·min^(-1),检测波长220 nm。结果 PAS-Na与已知杂质间氨基酚的线性范围均为0.02~2.0 mg·L^(-1)(r=0.9999,n=5),二者的检出限分别为0.050、0.068 ng;6批注射用PAS-Na样品中,间氨基酚的含量均<0.01%,最大单个未知杂质的含量均<0.01%,总杂质含量均<0.01%。结论所用方法可用于注射用PAS-Na中有关物质的测定。

OBJECTIVE To establish an ion - pair HPLC method for the determination of the related substances in Sodium aminosalicylate （PAS - Na） for injection. METHODS The determination was performed on a C18 column with the mobile phase composed of 0.05 mol·L-1 monobasic sodium phosphate （900 mL） ,and acetonitrile （100 mL） containing 10% tetrabutyl ammonium hydroxide at （0.2 g）. The flow rate was 1.0 mL·min-1 , and the detection wavelength was 220 nm. RESULTS A good linearity was obtained in the range of 0.2 - 2.0 mg·L - 1 （ r = 0. 99995, n = 5 ） for PAS - Na and 3 - aminophenol, where the LODs was 0. 050 ng and 0. 068 ng respectively. The contents of 3 - aminophenol in 6 batches of samples were all less than 0.01% , and the other maximum impurity was all less than 0.01%. The total amount of impurity was all less than 0.01%. CONCLUSION The method is suitable for the determination of the related substances in PAS - Na.