摘要
目的:建立双柱串联方式测定甘露醇有关物质的高效液相色谱-电喷雾检测器(HPLC-CAD)方法。方法:采用2根钙型阳离子交换柱SHODEX SUGAR SC1011(300 mm×8.0 mm)色谱柱串联的方式,柱温为80℃,水为流动相,流速为0.5 mL·min^(-1);雾化器温度:60℃,滤光片为10.0,采集频率:200 Hz,幂函数为1.15;进样体积20μL。结果:出峰顺序分别为异麦芽糖醇峰1、麦芽糖醇峰、异麦芽糖醇峰2、甘露醇峰、山梨醇峰,麦芽糖醇与异麦芽糖醇峰2分离度为1.2,其余各峰之间的分离度均大于1.5;以各物质浓度的自然对数对峰面积的自然对数建立标准曲线,r均>0.9992;精密度良好(RSD均<1.3%);加样回收率为97.3%~99.3%(RSD为1.1%~1.2%,n=9);检测限为2.0~3.7μg·mL^(-1),定量限为6.8~12.0μg·mL^(-1);样品测定结果与现行标准方法测定结果一致。结论:使用双柱串联后,麦芽糖醇峰和异麦芽糖醇峰2之间的分离度得到有效提高,优于现有国内外药典及文献方法;本方法准确、简便、可靠,可用于测定甘露醇有关物质。
Objective:To establish an HPLC-CAD method for the determination of mannitol related substances of mannitol with two columns in series.Methods:Two SHODEX SUGAR SC1011(300 mm×8.0 mm)columns were used in series,the column temperature was set at 80℃,water was used as mobile phase and the flow rate was 0.5 mL·min^(-1).The detector of CAD was applied with nebulization temperature at 80℃,filter frequency at 10.0,collection frequency at 200 Hz,and power function value(PFV)at 1.15.The injection volume was 20μL.Results:The peak order of mixed solution was isomalt peak 1,maltitol peak,isomalt peak 2,mannitol peak,sorbitol peak respectively,the resolution between maltitol and isomalt peak 2 was 1.2,and the resolution betweenthe other peaks was greater than 1.5.The linearity of the natural logarithm and the natural logarithm of the peak area of each substance was good(r>0.9992).The precision of injection was good(RSD<1.3%).The recovery was 97.3%-99.3%(RSD 1.1%-1.2%,n=9).The LOD was 2.0-3.7μg·mL^(-1)and the LOQ was 6.8-12.0μg·mL^(-1).The measurement results of the samples are consistent with those of the current standard method.Conclusion:The new established HPLC-CAD method shows better resolution of determination than that of existing methods and can make up for the defects of present pharmacopoeia methods,which can be a reliable method for the quality control of mannitol.
作者
谭菊英
梁秋霞
刘庄蔚
王娟
杨欣智
邓鸣
TAN Ju-ying;LIU Qiu-xia;LIU Zhuang-wei;WANG Juan;YANG Xin-zhi;DENG Ming(Guangxi Institute for Food and Drug Control,Nanning 530021,China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2022年第12期2129-2135,共7页
Chinese Journal of Pharmaceutical Analysis
基金
国家科技重大专项—重大新药创制“药物一致性评价关键技术与标准研究”(2017ZX09101001)
广西药品监督管理局2019年直属单位单位药品安全科研项目计划:化学药物关键质量属性分析方法研究[桂药监科2019-06(直属)]
广西药品监督管理局2020年直属单位单位药品安全科研项目计划:基于国家药品评价性抽验的化学药品质量控制体系的建立与应用[桂药监科2020-(直属)]。
