热解吸-气质联用法快速筛查和半定量分析医疗器械中增塑剂

Rapid Screening and Semi-quantitative Analysis of Plasticizers in Medical Devices by Thermal Desorption-gas Chromatography/mass Spectrometry

采用固体样品直接进样技术,利用裂解仪的热解吸功能,通过加热将待测样品中的增塑剂释放出来,并在线利用气质联用仪对释放出来的增塑剂进行定性和半定量分析,外标法定量,从而建立了1个快速筛查和半定量分析医疗器械中34种增塑剂的气质联用分析方法,对附件初始温度、热解吸温度、热解吸时间等裂解器热解吸工作条件以及仪器分析条件进行了优化,并研究了方法的线性关系和精密度。DINP和DIDP的检出限均为10 mg/kg,其余32种目标分析物的检出限为0.1~2.0 mg/kg,方法精密度实验的相对标准偏差(RSD, n=6)为2.16%~13.49%。由于该方法不使用任何有机溶剂进行前处理,不会产生环境污染,对环境友好。该方法简单快速、灵敏度高、定性可靠,检出限低,满足相关法规的限量要求,可完全满足医疗器械中增塑剂的日常检测工作需要。

Plasticizers in the samples to be tested was released by heating based on the thermal desorption function of the pyrolysis instrument,using the solid sample direct injection technology,then qualitative and semi-quantitative analysis of the released plasticizers were carried out on-line using the gas chromatography/mass spectrometry(GC/MS)technique.The concentration of each plasticizer was calibrated by the external standard method.Therefore,a GC/MS method was established for the rapid screening and semi-quantitative determination of 34 plasticizers in medical devices.The instrumental analysis conditions and the working conditions of thermal desorption such as initial temperature of the accessory,thermal desorption temperature and thermal desorption time were optimized.The linear relationship and precision of the method were also studied.The limits of detection(LODs)were all 10 mg/kg for DINP and DIDP.The limits of detection(LODs)of other 32 plasticizers varied from 0.1 mg/kg to 2.0 mg/kg.The relative standard deviation(RSD,n=6)varied from 2.16%to 13.49%.The proposed method needed no organic solvents for pretreatment,therefore,it caused no environmental pollution and was environmentally friendly.The proposed method was simple,rapid,sensitive and reliable to qualitative analysis.The limits of detection(LODs)were quite low and could meet the limitation requirements of relevant regulations,and could completely meet the demand on routine analysis of plasticizers in medicine devices.