注射用哌拉西林钠/三唑巴坦钠有关物质测定方法的研究  

Study on the determination method of related substances of piperacillin sodium and tazobactam sodium for injection

作　　者：姚兰 刘亚威 张亚杰 孙苓苓 Yao Lan;Liu Ya-wei;Zhang Ya-jie;Sun Ling-ling(Liaoning Institute for Drug Control,Shenyang 110032)

机构地区：[1]辽宁省药品检验检测院抗生素室,沈阳110032 [2]辽宁省药品检验检测院,沈阳110032

出　　处：《中国抗生素杂志》2020年第3期293-299,共7页Chinese Journal of Antibiotics

摘　　要：目的建立适合国内各生产企业注射用哌拉西林钠/三唑巴坦钠有关物质测定的方法。方法采用高效液相色谱法,色谱柱为Thermo Hypersil-ODS(4.6mm×25cm, 5μm);以乙腈-4g/L磷酸二氢钠溶液溶液(2:98)(用1mol/L氢氧化钠溶液调节pH值至6.0)为流动相A,以乙腈为流动相B,梯度洗脱;检测波长220nm;流速1.5mL/min。结果与中国药典2015年版所收载的有关物质检查法比较,梯度洗脱方法提高了杂质检出能力,共检出14个已知杂质,杂质分离完全,杂质谱更加完整,能够同时控制二聚体等聚合物杂质。经方法学验证,各杂质在线性范围内线性关系良好,回收率结果方法准确可靠。结论该方法能够全面的反应本品的杂质情况,适合国内各企业样品的检测。Objective To establish a method for the determination of related substances of piperacillin sodium and tazobactam sodium for injection of domestic production. Methods High performance liquid chromatography was used. The column was Thermo Hypersil-ODS(4.6 mm×25 cm, 5μm). Acetonitrile-4 g/L sodium dihydrogen phosphate solution(2:98, the pH value was adjusted with 1 mol/L sodium hydroxide solution to 6.0) was mobile phase A, with acetonitrile as mobile phase B. The gradient elution method was used. The detection wavelength was 220 nm. Flow rate was 1.5 mL/min. Results Compared with the method contained in the ChP 2015, the gradient elution method improved the impurity detection ability, and 14 known impurities were detected. The impurities were completely separated and the impurity list was more complete. Polymer impurities such as dimers were controlled. According to the methodological verification, the linear relationship of each impurity in the linear range was good, and the recovery result was accurate and reliable. Conclusion This method can comprehensively reflect the impurity of the product, and is suitable for the detection of samples from domestic enterprises.

关 键 词：注射用哌拉西林钠/三唑巴坦钠 有关物质 梯度洗脱 

分 类 号：R978.1[医药卫生—药品] R917[医药卫生—药学]