电喷雾萃取电离-三重四极杆质谱快速检测PVC医疗器械中残留环己酮的方法研究
收稿日期: 2015-04-10
网络出版日期: 2015-07-07
基金资助
项目受国家自然科学基金(Nos. 21477132, 81401756), 国家科技支撑计划(No. 2015BAI01B04), 安徽省科技攻关项目(No. 1301042095)和合肥物质科学技术中心创新项目培育基金(No. 2014FXCX007)资助.
Rapid Analysis of Residual Cyclohexanone in PVC Infusion Set by Extractive Electrospray Ionization-Mass Spectrometer/Mass Spectrometer
Received date: 2015-04-10
Online published: 2015-07-07
Supported by
Project supported by the National Natural Science Foundation of China (Nos. 21477132, 81401756), the National Key Technology Research and Development Program of the Ministry of Science and Technology of China (No. 2015BAI01B04), the Anhui Provincial Program for Science and Technology Development, China (No. 1301042095) and the Innovative Program of Development Foundation of Hefei Center for Physical Science and Technology, China (No. 2014FXCX007).
环己酮是一种广泛使用在PVC医疗器械生产中的粘接剂, 残留的环己酮会通过输液或介入治疗等过程进入人体而产生潜在危害, 快速检测残留环己酮对PVC医疗器械的质量控制具有重要意义. 结合三重四极杆质谱和电喷雾萃取电离技术, 建成能够对痕量环己酮气体快速检测的电喷雾萃取电离-三重四极杆质谱仪(EESI-MS/MS). 通过对EESI电离源的喷雾电压、载气流速等条件进行优化, 得到最优喷雾电压为3000 V, 最佳载气流速为11.67 L/min, 装置响应时间小于2.5 s, 信号强度的相对标准偏差为4.83%, 仪器的检出限为237.1×10-9 (V/V). 利用EESI-MS/MS实现了对PVC输液管中残留环己酮的快速检测, 配合串级质谱的子离子扫描功能实现了环己酮的准确定性, 同时计算得到PVC输液管中残留环己酮的浓度为362.6×10-9 (V/V). 建立的EESI-MS/MS在PVC医疗器械质量控制方面具有重要的应用价值.
关键词： PVC输液管; 电离源; 电喷雾萃取电离-三重四极杆质谱; 环己酮; 快速检测
邹雪 , 王鸿梅 , 陆燕 , 黄超群 , 夏磊 , 陈小景 , 沈成银 , 储焰南 . 电喷雾萃取电离-三重四极杆质谱快速检测PVC医疗器械中残留环己酮的方法研究[J]. 化学学报, 2015 , 73(8) : 851 -855 . DOI: 10.6023/A15040250
Cyclohexanone is widely used as adhesive in the production of PVC medical devices. Residual cyclohexanone in PVC medical devices may enter into human body through transfusion or intervention treatment, which can cause potential harm to human body. Therefore, rapid detection of the residual cyclohexanone is important to quality control of PVC medical devices. Based on the conventional electrospray ionization mass spectrometer/mass spectrometer (ESI-MS/MS), an extractive electrospray ionization mass spectrometer/mass spectrometer (EESI-MS/MS) for detection of trace cyclohexanone gas was built. The EESI technique can directly analyze the gas and liquid samples without pre-treatment, and the tandem mass spectrometry can unambiguously identify ions with the scan mode of product ions. To improve the performance of the instrument, effective parameters for rapid detection of cyclohexanone were optimized first of all. Laboratory air as sample, spray voltage of EESI was optimized to be 3000 V; Standard acetone gas as sample, carrier gas flow was optimized to be 11.67 L/min. And then the performance of the EESI-MS/MS was evaluated. The standard acetone gas was used as sample to test response time and repeatability (n=6) of the apparatus. The result showed that the response time of this EESI-MS/MS was less than 2.5 s, providing a real-time detection. And on the basis of 6 injections of the same sample, relative standard deviation (RSD) of signal intensities for acetone was 4.83%. A calibration curve was lined and the (limit of detection) LOD of the instrument was calculated to be 237.1×10-9 (V/V) with (signal/noise) S/N=3. Finally, EESI-MS/MS was used for fast detection of residual cyclohexanone gas in PVC infusion set. Comparing the mass spectra of standard cyclohexanone gas and air in the PVC infusion set, we found they all contained ions at m/z 99 and m/z 81. MS/MS technology was then used to make further investigation of the origin of the ions at m/z 99 from the air in the PVC infusion set and the production procedure of m/z 81. In detail, product ions' mass spectra of cyclohexanone gas and air in the PVC infusion set was compared when collision energy was set to be 5, 10, and 15 eV. At each collision energy, product ions' mass spectrum of air in PVC infusion set was same to that of cyclohexanone gas. So it can be sure that the air in PVC infusion set contained cyclohexanone. Ion m/z 81 was produced from the fragmentation of protonated cyclohexanone. In addition, the concentration of the cyclohexanone in the PVC infusion set can be calculated to be 362.6×10-9 (V/V). The result shows the important application value of EESI-MS/MS in quality control of medical devices.
Key words： PVC infusion set; ion source; EESI-MS/MS; cyclohexanone; fast detection
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