北京生物医学工程

全降解冠脉雷帕霉素洗脱支架系统有机溶剂残留分析

Analysis of residual organic solvents in biodegradable coronary rapamycin-eluting stents

作者：王丽付步芳魏嫣史国华杨光王春仁

单位：                                 河北省医疗器械与药品包装材料检验研究院(石家庄050061)            

关键词：气相色谱；质谱；顶空进样；全降解；支架；有机溶剂

分类号：

出版年·卷·期（页码）：2015·34·4（398-402）

摘要：

目的采用顶空进样-气相色谱-质谱联用法（headspace sampling-gas chromatography-mass spectrometry, HS-GC-MS）测试全降解冠脉雷帕霉素洗脱支架系统有机溶剂残留的情况，最终建立顶空进样-气相色谱-氢火焰离子化检测器( headspace sampling-gas chromatography-flame ionization detector, HS-GC-FID）定量测定丙酮残留量的检测方法。方法采用HS-GC-MS，全扫描模式对全降解支架系统中的含药支架、球囊、输送系统、支架原料及裸支架5种被测对象进行残留有机溶剂的定性分析，并采用HS-GC-FID对其中残留较多的丙酮进行了定量分析。结果 5种被测对象中均有多种有机溶剂残留，主要为芳香烃类(甲苯)、酮类(丙酮)、卤化烃类（二氯甲烷、三氯甲烷）、醇类（乙醇等）、酯类（乙酸乙酯等）。丙酮在9.0～44.8 μg/mL浓度范围内线性良好，相关系数为0.9995，平均加样回收率为100.3% (n=6, RSD=1.2%) ，精密度为2.0%（n=5）。结论新产品注册检测含药支架有机溶剂残留的同时，建议考察支架原料、裸支架的有机溶剂残留。建立的定量检测方法简便、快速、准确，可用于全降解支架系统中残留有机溶剂的检测与质量控制。

Objective To measure the residual organic solvents in biodegradable coronary rapamycin-eluting stents using HS-GC-MS and to establish an HS-GC-FID method for the determination of residual acetone in biodegradable coronary rapamycin-eluting stents. Methods A full scan mode of HS-GC-MS was used to analyze the residual organic solvents in the rapamycin-eluting stent, the balloon, the delivery system, raw materials and the bare stent, respectively, and the acetone content in the rapamycin-eluting stent was determined using HS-GC-FID. Results Certain organic solvents were observed, including aromatic hydrocarbon (toluene), ketone (acetone), halogenated hydrocarbons (methylene chloride and chloroform), alcohols (ethanol, etc.) and esters (ethyl acetate, etc.). The linear range of acetone was 9.0 to 44.8μg/mL (r=0.9995). The average recovery rate was 100.3% (n=6, RSD=1.2%) and the precision was 2.0% (n=5). Conclusions The residual organic solvents in rapamycin-eluting stents, the raw materials and the bare stents should be investigated during the registration evaluation of the biodegradable coronary rapamycin-eluting stents. The quantitative analysis is rapid, accurate and convenient. It is suitable for the determination of the residual organic solvents in biodegradable coronary rapamycin-eluting stents.

参考文献：

［1］Rasal RM, Janorkar AV, Hirt DE. Poly(lactic acid) modifications［J］.Progress in Polymer Science,2010,35（3）：338-356.
［2］Zilberman M, Schwade ND, Eberhart RC. Protein-loaded bioresorbable fibers and expandable stents：Mechanical properties and protein release［J］. J Biomed Mater Res B Appl Biomater, 2004, 69（1）：1-10.
［3］Li SM, Vert M. Biodegradable polymers：polyesters［M］// Mathiowitz E. Encyclopedia of Controlled Drug Delivery. Hoboken：John Wiley & Sons, 1999: 71-93.
［4］Zidar J, Lincoff AM, Stack R. Biodegradable stents［M］// Topol EJ.Textbook of Interventional Cardiology. 2nd ed. Philadelphia, PA：W.B. Saunders, 1994: 787-802.
［5］National Pharmacopoeia Committee.Pharmacopoeia of the People’s Republic of China ［M］. Beijing:Chemical Industry Press,2010:Appendix Ⅷ p:61-65.

服务与反馈：

【文章下载】【加入收藏】

提示：您还未登录，请登录！点此登录