氟[^(18)F]脱氧葡糖注射液中未知杂质三甲基硅醇的研究  

Unknown Impurities Trimethylsilanol in Fludeoxyglucose[^(18)F]Injection

作　　者：贾娟娟[1] 孙得洋 程茗 施亚琴[1] 弓全胜 张文在 JIA Juanjuan;SUN Deyang;CHENG Ming;SHI Yaqin;GONG Quansheng;ZHANG Wenzai(National Institutes for Food and Drug Control,NMPA Key Lab for Quality Research and Chemical Drug,Beijing 102629,China)

机构地区：[1]中国食品药品检定研究院,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,北京102629

出　　处：《同位素》2023年第2期198-202,I0004,共6页Journal of Isotopes

摘　　要：为确定氟[^(18)F]脱氧葡糖注射液残留溶剂测定中未知成分的结构和来源,采用气相色谱-质谱联用(GC-MS)分析^(18)F-FDG样品,结果显示,主要的未知杂质成分为三甲基硅醇,来源于制备过程中固相碱水解工艺C18柱封端填料的降解。采用气相色谱法测定三甲基硅醇的含量,方法学验证结果符合要求,线性范围为0.003~1.5 mg/mL,相关系数为0.9991;检测限和定量限分别为0.001 mg/mL、0.003 mg/mL。对56批含三甲基硅醇的样品进行测定,结果显示三甲基硅醇含量为0.003~0.380 mg/mL。研究结果显示,残留溶剂测定中的未知成分并无机溶剂,建议改进制备工艺,避免引入色谱柱填料的降解杂质。To investgate the structure and source of unknown components in the residual solvent,Fludeoxyglucose[^(18)F]injection was analyzed by GC-MS.The results indicated that the main unknown impurity was trimethylsilanol which came from the degradation of backing material in C18 column during the on-column basic hydrolysis process.The content of trimethylsilanol was determined by GC,and the method validation results met the requirements.The linear range was from 0.003 mg/mL to 1.5 mg/mL,and the correlation coefficient was 0.9991.The limits for detection and quantitation were 0.001 mg/mL and 0.003 mg/mL respectively.56 batches of^(18)F-FDG samples containing trimethylsilanol were measured,and the concentration of trimethylsilanol was from 0.003 mg/mL to 0.380 mg/mL.The results show that the unknown components in the residual solvent determination are not organic solvent residues.It is suggested that the preparation process should be improved to avoid the impurities from the column packing degradation.

关 键 词：氟[^(18)F]脱氧葡糖注射液 气相色谱-质谱联用 杂质 三甲基硅醇 

分 类 号：TL923[核科学技术—核燃料循环与材料]