摘要
目的建立一种检验生物检材中无机氰化物的GCMS／MS方法。方法首先将生物检材中的无机氰化物在酸性条件下蒸馏出，用碱性溶液吸收后，氰离子在相转移催化剂作用下被五氟苄基溴（PFB-Br）衍生化，最后用GC-MS／MS法分析衍生化产物。结果衍生化产物PFB-CN的MS／MS质谱图特征性强，定性准确；在20-1500ng／g浓度范围内呈良好的线性关系（r＝0．998），最低检测限为5ng／g，回收率为82．3％－98．6％。结论本方法简单实用，灵敏度高，准确可靠，适用于生物检材中无机氰化物的检验。
Objective To establish a GC-MS/MS method for the determination of inorganic cyanide in biological samples. Method Inorganic cyanide in biological samples was separated by distillation under acid condition, and absorbed by alkaline solutions. Then the cyanide ion was derivatized by pentafluorobenzyl bromide （PFB-Br） with the use of a phase transfer catalyst, the derivative was detected by GC-MS/MS finally. Results The MS/MS spectrum of PFB-CN was characteristic, and the qualitative analysis was accurate. The linear range of PFB-CN was 20 to 1500 ng/g （r=0. 998）, the lowest detectable limit was less than 5 ng/g. The method recovery was 82.3% to 98. 6%. Conclusion The method is simple and sensitive, the analytical results are reliable and accurate. It can be used effectively for the determination of inorganic cyanide in biological samples.
出处
《刑事技术》
2009年第6期31-34,共4页
Forensic Science and Technology
