Tsujita Akira, Okazaki Hidehiko, Nagasaka Asami, Gohda Akinaga, Matsumoto Mitsushi, Matsui Toshiro
Forensic Science Laboratory, Fukuoka Prefectural Police Headquarters, 7-7 Higashikoen, Fukuoka, 812-8576 Japan.
2Department of Bioscience and Biotechnology, Faculty of Agriculture, Graduate School of Kyushu University, 744 Motooka, Fukuoka, 819-0395 Japan.
Forensic Toxicol. 2019;37(1):75-81. doi: 10.1007/s11419-018-0437-6. Epub 2018 Aug 13.
In this study, we proposed a new sensitive quantitative method for detecting helium in human blood by gas chromatography-selected-ion monitoring (SIM)-mass spectrometry (GC-SIM-MS) using naturally existing neon-21 in air as internal standard (IS).
GC-SIM-MS analysis was performed on a double TC-Molsieve 5A capillary column (total length 60 m) for the separation of permanent gases by a single-run experiment. By using hydrogen as the carrier gas, the analyte (helium) and IS (neon-21) were separated on the double column, and detected at 4 and 21, respectively. The ratio of the peak area of helium-to-neon-21 was used for obtaining the calibration curve for helium determination.
The limits of detection and quantification of helium under the present GC-SIM-MS conditions were as low as 1.8 and 6.0 ppm, respectively. The proposed GC-SIM-MS method also showed high repeatability with relative standard deviation at 1.3-5.1%, indicating that the use of neon-21 as IS was valid for reliable helium assays. The successful quantification of helium in the headspace of vacuum blood collection tubes containing the whole blood from four humans who died of helium inhalation was achieved using the proposed neon-21-aided GC-SIM-MS method; the values obtained for helium were 24-497 ppm.
The proposed GC-SIM-MS method in combination with the naturally existing neon-21 as IS is most recommendable for quantitative assays of helium in biological samples because of its simplicity and extremely high sensitivity.
在本研究中,我们提出了一种新的灵敏定量方法,通过气相色谱 - 选择离子监测(SIM)-质谱联用(GC-SIM-MS),以空气中天然存在的氖 - 21作为内标(IS)来检测人体血液中的氦气。
采用双TC - 分子筛5A毛细管柱(总长度60 m)进行GC-SIM-MS分析,通过单次运行实验分离永久性气体。以氢气作为载气,分析物(氦气)和内标(氖 - 21)在双柱上分离,并分别在质荷比4和21处进行检测。氦气与氖 - 21的峰面积比用于获得氦气测定的校准曲线。
在当前GC-SIM-MS条件下,氦气的检测限和定量限分别低至1.8 ppm和6.0 ppm。所提出的GC-SIM-MS方法还显示出高重复性,相对标准偏差为1.3 - 5.1%,表明使用氖 - 21作为内标对于可靠的氦气检测是有效的。使用所提出的氖 - 21辅助GC-SIM-MS方法成功定量了四名死于氦气吸入的人类全血真空采血管顶空中的氦气;获得的氦气值为24 - 497 ppm。
所提出的GC-SIM-MS方法结合天然存在的氖 - 21作为内标,因其简单性和极高的灵敏度,最推荐用于生物样品中氦气的定量测定。