PTA球囊扩张导管中2-氯乙醇残留量的评价方法

目的建立气相色谱-质谱(GC-MS)联用的方法分析ECH残留量,以便对PTA球囊扩张导管中的ECH残留量水平进行安全性评价。方法以丙酮为溶剂,超声提取样品中的2-氯乙醇。色谱柱ZB-624,进样口温度180℃,分流比1∶1,载气为高纯He,流速1.5 g/m L。升温条件:50℃(1 min),5℃/min升至100℃。质谱条件:离子源温度230℃,接口温度250℃,电子能量70 e V。以保留时间和质谱全扫描方式进行定性分析,质荷比m/z 35~500。选择离子监测模式外标法定量,定量离子m/z=43。结果该方法理论塔板数在56753以上,在1.44~22.96μg/m L浓度范围,线性关系良好,r=0.999,平均加样回收率为99.1%(n=5,RSD5%),检出限为0.41μg/m L。样品中未检出ECH残留。结论建立的基于GC-MS的2-氯乙醇残留量的分析方法灵敏、快速、准确,可供企业对PTA球囊扩张导管产品的质量控制和检测同行参考。

Evaluation method of residual ethylene chlorohydrin in PTA balloon dilatation catheter

Objective To develop a gas chromatography-mass spectrometric ( GC-MS ) method for the determination and evaluation of ethylene chlorohydrin ( ECH ) residue in PTA balloon dilatation catheter. Methods The ECH residue were extracted in acetone by ultrasonic bathing. Chromatographic column ZB-624, inlet temperature 180 ℃, split ratio 1 : 1, high purity He as carrier gas, column flow rate 1. 5 mL/min. Temperature programmed condition:50℃ (1min),5℃/min to 100℃. Mass spectrometric conditions were as follow:ion source temperature 230 ℃, the interface temperature between GC and MS was 250 ℃, electrical energy 70 eV. Qualitative analysis was carried out by retention time and mass spectrometric scan,m/z between 35 and 500,and quantified by select ion monitoring method ( SIM ) , m/z=43. The ECH was determined by external standard method under the SIM mode by GC-MS. Results The number of theoretical plates were more than 56753. A good linearity was obtained at the concentrations of 1. 44～22. 96μg/mL with a correlation of 0. 999 and the average recovery was 99. 1％ ( n=5,RSD<5％) . The minimum limit of ECH was 0. 41μg/mL. No ECH was found in the sample. Conclusions The method of GC-MS is sensitive, rapid and accurate for determination of ECH residue in PTA balloon dilatationcatheter products. It can be used for quality control of PTA balloon dilatation catheter and for peers reference.