核磁共振氢谱法测定注射用微球专用溶剂中硅油的含量  

Determination of Silicone Oil in Diluent for Suspension of Microspheres for Injection by Nuclear Magnetic Resonance

作　　者：马佳慧 夏昀卿 沈莉 薛英 周凤梅 刘万卉[1] 许丽晓 Ma Jiahui;Xia Yunqing;Shen Li;Xue Ying;Zhou Fengmei;Liu Wanhui;Xu Lixiao(School of Pharmacy,Key Laboratory of Molecular Pharmacology and Drug Evaluation(Yantai University),Ministry of Education,Collaborative Innovation Center of Advanced Drug Delivery System and Biotech Drugs in Universities of Shandong,Yantai University,Yantai 264005,China;National Key Laboratory of Advanced Drug Delivery and Release Systems,Shandong Luye Pharmaceutical Co.,Ltd.,Yantai 264003,China)

机构地区：[1]烟台大学药学院新型制剂与生物技术药物研究山东省高校协同创新中心分子药理和药物评价教育部重点实验室(烟台大学),山东烟台264005 [2]山东绿叶制药有限公司先进药物递释系统全国重点实验室,山东烟台264003

出　　处：《山东化工》2024年第3期138-140,145,共4页Shandong Chemical Industry

基　　金：山东省高等学校科技计划(J18KA275)。

摘　　要：目的:建立测定注射用微球专用溶剂中硅油含量的定量核磁共振氢谱(qHNMR)法。方法:采用Bruker Avance NEO 600型核磁共振波谱仪测定核磁共振氢谱(^(1)H NMR),脉冲序列zg30,弛豫延迟时间15 s,采样次数16,测定温度25℃,以咖啡因为内标,不加四甲基硅烷(TMS)的氘代氯仿为溶剂,对注射用微球专用溶剂中的硅油进行定量研究,以硅油定量峰与内标定量峰面积之比对其含量(μg)绘制标准曲线,计算注射用微球专用溶剂中硅油含量。结果:硅油含量在6~100μg范围内线性关系良好,r=0.9999,低、中、高浓度的平均回收率为97.8%(n=9),重复性RSD为9.8%。结论:该方法操作简单快捷、灵敏度高、结果准确,可用于注射用微球专用溶剂中硅油含量的测定。Objective:To establish a quantitative proton magnetic resonance(qHNMR)method for determination of silicone oil content in the diluent for suspension of microspheres for injection.Methods:The qHNMR were obtained in chloroform-d(without tetramethylsilane)with the internal standard caffeine by a Bruker Avance NEO 600 NMR spectrometer.The parameters of which were set up as follows:the pulse sequence was zg30,the relaxation delay time was 15 s,the number for scanning was 16,and the experiment temperature was controlled at 25℃.The assay of silicone oil was calculated by establishing a standard curve based on the ratio between the quantitative peak areas of silicone oil and the quantitative peak areas of the internal standard with the content of silicone oil.Results:The calibration curve was linear in the concentration range of 6~100μg with the correlation coefficient(r)of 0.9999.The average recovery at low,medium and high concentrations was 97.8%(n=9).And the reproducible RSD was 9.8%.Conclusion:The established method for the determination of silicone oil content in the diluent for suspension of microspheres for injection by using qHNMR is relatively convenient and simple,rapid,with high accuracy and sensitivity.

关 键 词：定量核磁共振氢谱法 注射用微球专用溶剂 硅油 含量测定 标准曲线法 

分 类 号：O657.2[理学—分析化学]