高效液相色谱-电喷雾检测器法测定程序性死亡蛋白-1抑制剂中甘露醇含量  

Determination of Mannitol in Programmed Death-1 Inhibitor by HPLC-CAD

作　　者：田沛霖 李玥琦 王思渊 鲁辉 张国林 TIAN Peilin;LI Yueqi;WANG Siyuan;LU Hui;ZHANG Guolin(Suzhou Institute for Drug Control,Suzhou,Jiangsu,China 215104)

机构地区：[1]江苏省苏州市药品检验检测研究中心,江苏苏州215104

出　　处：《中国药业》2022年第11期63-66,共4页China Pharmaceuticals

基　　金：江苏省苏州市科技计划项目[SYS2020199,SS202040]。

摘　　要：目的建立测定程序性死亡蛋白(PD-1)抑制剂中甘露醇含量的高效液相色谱-电喷雾检测器(HPLC-CAD)法。方法色谱柱为Supelco apHera NH_(2)氨基分析柱(150 mm×2 mm,5μm),流动相为乙腈-水溶液(80∶20,V/V),流速为1.0 mL/min,柱温为40℃,进样量为3μL。CAD雾化室温度为50℃,幂率为1.0,采样频率为10 Hz,过滤常数为5.0 s。结果甘露醇质量浓度在0.125~1.000 mg/mL范围内与峰面积线性关系良好(r=0.9973,n=5);精密度、稳定性均良好;检测限和定量限分别为0.200μg/mL和0.625μg/mL;平均回收率为95.31%,RSD为1.01%(n=6)。结论该方法操作简单、灵敏度高、检测迅速、结果准确,可用于PD-1抑制剂中甘露醇的含量测定。Objective To establish a high-performance liquid chromatography-charge aerosol detection(HPLC-CAD)method for the determination of mannitol in the programmed death-1(PD-1)inhibitor.Methods The chromatographic column was Supelco apHera NH_(2) amino analysis column(150 mm×2 mm,5μm),the mobile phase was acetonitrile aqueous solution(80∶20,V/V),the flow rate was 1.0 mL/min,the column temperature was 40℃and the injection volume was 3μL.The detector of CAD was applied with the nebulization temperature of 50℃,power function value(PFV)of 1.0,collection frequency of 10 Hz and filtration constant of 5.0 s.Results The linear range of mannitol was 0.125-1.000 mg/mL(r=0.9973,n=5).The results of precision and stability tests were good.The limit of detection(LOD)and limit of quantitation(LOQ)were 0.200μg/mL and 0.625μg/mL,respectively.The average recovery of mannitol was 95.31%with an RSD of 1.01%(n=6).Conclusion The established method is simple,sensitive,rapid and accurate,which can be used for the determination of mannitol in the PD-1 inhibitor.

关 键 词：程序性死亡蛋白-1抑制剂 甘露醇 高效液相色谱法 电喷雾检测器 含量测定 

分 类 号：R979.5[医药卫生—药品] R927.2[医药卫生—药学]