吡拉西坦氯化钠注射液有关物质的测定及影响因素考察  

Determination of Related Substances in Piracetam and Sodium Chloride Injection and Investigation of Influencing Factors

作　　者：张迪 张丽 李尚颖 徐万魁 ZHANG Di;ZHANG Li;LI Shang-ying;XU Wan-kui(Liaoning Inspection,Examination and Certification Centre,Liaoning Shenyang,China 110036;Liaoning Institute for Drug Control/NMPA Key Laboratory for Quality Research and Evaluation of Chemical Drug,Liaoning Shenyang 110036,China)

机构地区：[1]辽宁省检验检测认证中心,辽宁沈阳110036 [2]辽宁省药品检验检测院/国家药品监督管理局化学药品质量研究与评价重点实验室,辽宁沈阳110036

出　　处：《中国药物评价》2024年第3期192-197,共6页Chinese Journal of Drug Evaluation

基　　金：辽宁省科学技术计划基金项目(No.2020-MS-074)。

摘　　要：目的:建立测定吡拉西坦氯化钠注射液中有关物质的方法,并考察相关影响因素。方法:采用高效液相色谱法检测,用十八烷基硅烷键合硅胶为填充剂(DIKMA Platisil ODS 5μm 250×4.6 mm),以含0.1%磷酸氢二钾的水溶液(用50%磷酸调节pH至6.0)为流动相A,以乙腈为流动相B,梯度洗脱,流速为1.0 mL·min^(-1),柱温为35℃,检测波长为210 nm,进样量为10μL。结果:吡拉西坦及杂质A、B、C、D的线性范围分别为0.2552~1.0208、0.2458~0.9832、0.2527~1.0108、0.2589~1.0356、0.2451~0.9804μg·mL^(-1),各杂质的校正因子分别为1.3、1.3、1.5、0.8;检测限分别为3.527、10.304、30.554、1.981 ng·mL^(-1),定量限分别为8.817、25.760、76.384、4.952 ng·mL^(-1),回收率为90.18%~105.2(RSD为1.5%~3.3%,n=9)。吡拉西坦氯化钠注射液在贮存过程中,有降解趋势,杂质D为主要降解产物,温度越高,降解速度越快。结论:建立的方法可准确测定吡拉西坦氯化钠注射液中有关物质的含量,专属性好,灵敏度高,影响吡拉西坦氯化钠注射液有关物质的主要因素为温度和贮存时间,企业应注意灭菌条件的选择,同时在整个流通环节,注意控制并监控好贮存温度,以保证产品的质量和安全。Objective:To establish a method for the determination of related substances in Piracetam and sodium chloride injection,and to investigate the influence of related factors.Methods:High Performance Liquid Chromatography(HPLC)was performed on an octadecylsilane bonded silica gel column(DIKMA Platisil ODS 5μm 250×4.6 mm),The mobile phase was Dipotassium phosphate solution(pH to 6.0 with 50%phosphoric acid)/acetonitrile in a gradient elution.The flow rate was 1.0 mL·min-1.Column temperature was 35℃.The detection wavelength was 210 nm.Injection volume was 10μL.Results:The linear ranges of Piracetam and impurities A,B,C,D were 0.2552-1.0208,0.2458-0.9832,0.2527-1.0108,0.2589-1.0356,0.2451-0.9804μg·mL^(-1).The correction factors of the 4 impurities were 1.3,1.3,1.5 and 0.8.The detection limits were 3.527,10.304,30.554,1.981 ng·mL^(-1)respectively.The quantification limits were 8.817,25.760,76.384,4.952 ng·mL^(-1)respectively.The recoveries were 90.18%-105.20%(RSD=1.5%-3.3%,n=9).There was a tendency of degradation during the storage of Piracetam sodium chloride injection.Impurity D is the main degradation product.The higher the temperature is,the faster the degradation rate is.Conclusion:The established method can accurately determine the related substances in Piracetam sodium chloride injection with good specificity and high sensitivity.The main factors affecting the related substances in Piracetam sodium chloride injection are temperature and storage time,enterprises should pay attention to the selection of sterilization conditions,and control and monitor the storage temperature in the whole circulation to ensure product quality and people′s safety.

关 键 词：吡拉西坦氯化钠注射液 有关物质 高效液相色谱法 稳定性 影响因素 

分 类 号：R927.2[医药卫生—药学]