CAJ | 학술논문

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9.0~44.8μg / 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。
목적：채용정공진양-기상색보-질보련용법（ headspace sampling-gas chromatography-mass spectrometry，HS-GC-MS）측시전강해관맥뢰파매소세탈지가계통유궤용제잔류적정황，최종건립정공진양-기상색보-경화염리자화검측기（ headspace sampling-gas chromatography-flame ionization detector， HS-GC-FID）정량측정병동잔류량적검측방법。방법채용 HS-GC-MS，전소묘모식대전강해지가계통중적함약지가、구낭、수송계통、지가원료급라지가5충피측대상진행잔류유궤용제적정성분석，병채용HS-GC-FID 대기중잔류교다적병동진행료정량분석。결과5충피측대상중균유다충유궤용제잔류，주요위방향경류（갑분）、동류（병동）、서화경류（이록갑완、삼록갑완）、순류（을순등）、지류（을산을지등）。병동재9.0~44.8μg / mL 농도범위내선성량호，상관계수위0.9995，평균가양회수솔위100.3%（n =6，RSD =1.2%），정밀도위2.0%（n =5）。결론신산품주책검측함약지가유궤용제잔류적동시，건의고찰지가원료、라지가적유궤용제잔류。건립적정량검측방법간편、쾌속、준학，가용우전강해지가계통중잔류유궤용제적검측여질량공제。
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. 8 μg / 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.