HPLC测定吡拉西坦注射液有关物质的方法  

Determination of Related Substances of Piracetam Injection by HPLC

作　　者：钱锦花 朱琼瑶 吴燕娟 Qian Jinhua;Zhu Qiongyao;Wu Yanjuan(Guangdong Sunho Pharmaceutical Co.,Ltd.,Zhongshan 528437,China)

机构地区：[1]广东星昊药业有限公司,广东中山528437

出　　处：《广东化工》2023年第21期135-137,共3页Guangdong Chemical Industry

摘　　要：目的:建立HPLC测定吡拉西坦注射液有关物质方法。方法:采用十八烷基硅烷键合硅胶为填充剂,以磷酸盐缓冲液(1.0 g/L磷酸氢二钾溶液,用磷酸调节pH值为6.0):甲醇(90∶10)为初始比例,进行梯度洗脱,检测波长210 nm,流速1.0 mL/min,柱温30℃,进样体积10μL。结果:吡拉西坦峰与相邻杂质峰能较好地分离,吡拉西坦、杂质A、杂质B、杂质C和杂质D浓度分别在0.2555~1.0220μg/mL(r=0.9999)和0.2555~5.1100μg/mL(r=1.0000)、0.2610~1.0439μg/mL(r=0.9992,校正因子为1.7)、0.2519~1.0074μg/mL(r=0.9999,校正因子为1.4)、0.2528~1.0112μg/mL(r=0.9993,校正因子为1.3)、0.2494~4.9882μg/mL(r=1.0000,校正因子为0.67)范围内与峰面积呈良好的线性关系;吡拉西坦、已知杂质(杂质A、杂质D)的平均回收率分别为:99.3%~101.0%、96.1%~100.3%、99.9%~100.1%,RSD依次为:0.87%、2.9%、0.35%(n=9)。结论:本方法专属性强、准确、灵敏,可用于吡拉西坦注射液的有关物质检测和质量控制。Objective:To establish an HPLC method for the determination of related substances of Piracetam injection.Method:The chromatographic column was end-capped octadecylsilyl silica gel column.Gradient elution was performed with phosphate buffer(1.0 g/L dipotassium hydrogen phosphate solution,pH adjusted to 6.0 by phosphoric acid)and methanol(90∶10)as the initial ratio.The detection wavelength was 210 nm,the flow rate was 1.0 mL·min-1,the column temperature was 30℃,and the injeciton volumn is 10μL.Results:Piracetam peak and adjacent impurity peaks can be separated well,the linearity of Piracetam is good at the range from 0.2555μg/mL to 1.0220μg/mL(r=0.9999),the linearity of Piracetam is good at the range from 0.2555μg/mL to 5.1100μg/mL(r=1.0000),the linearity of Impurity A is good at the range from 0.2610μg/mL to 1.0439μg/mL(r=0.9992,the correction factor is 1.7),the linearity of Impurity B is good at the range from 0.2519μg/mL to 1.0074μg/mL(r=0.9999,the correction factor is 1.4),the linearity of Impurity C is good at the range from 0.2528μg/mL to 1.0112μg/mL(r=0.9993,the correction factor is 1.3),the linearity of Impurity D is good at the range from 0.2494μg/mL to 4.9882μg/mL(r=1.0000,the correction factor is 0.67).The average recovery of Piracetam,Impurity A and Impurity B is 99.3%~101.0%,96.1%~100.3%,99.9%~100.1%,respectively,and the RSD was 0.87%,2.9%,0.35%(n=9),respectively.Conclusion:The method is specific,accurate and sensitive,can be used for the determination and quality control of Piracetam Injection.

关 键 词：吡拉西坦注射液 有关物质 杂质检测 质量控制 高效液相色谱法 

分 类 号：R917[医药卫生—药物分析学]