PTA球囊扩张导管中2-氯乙醇残留量的评价方法

Evaluation method of residual ethylene chlorohydrin in PTA balloon dilatation catheter

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,RSD<5%),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。

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 m L/min.Temperature programmed condition： 50 ℃（ 1 min）,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 e V. Qualitative analysis was carried out by retention time and mass spectrometric scan,m/z between35 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. 96 μg/m L with a correlation of0. 999 and the average recovery was 99. 1%（ n = 5,RSD5%）. The minimum limit of ECH was 0. 41 μg/m L. 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 dilatation catheter products. It can be used for quality control of PTA balloon dilatation catheter and for peers reference.