扩散-吸收提取/离子色谱法检验血中氰化物  

Determination of cyanide in blood by ion chromatography with diffusion-absorption extraction

作　　者：吕惊晗 周晋升 宋丽娟[2] 郭杰[1] 石辉丽 蒋华宇 LYU Jinghan;ZHOU Jinsheng;SONG Lijuan;GUO Jie;SHI Huili;JIANG Huayu(Qingdao Municipal Public Security Bureau,Qingdao 266001,Shandong,China;Shandong Provincial Center for Physical Evidence Appraisal and Research,Jinan 250000,China)

机构地区：[1]青岛市公安局,山东青岛266001 [2]山东省公安厅物证鉴定研究中心,济南250000

出　　处：《化学分析计量》2024年第10期23-27,44,共6页Chemical Analysis And Meterage

基　　金：山东省重点研发计划(重大科技创新工程)项目(2021CXGC011305)。

摘　　要：建立扩散-吸收提取/离子色谱法检验血中氰化物。取1.0 mL血样置于10 mL顶空瓶中,加入1.0 mL超纯水混匀,再加入0.5 mL浓磷酸,放入装有0.5 mL 0.25%NaOH溶液的2.0 mL进样瓶中,密封后于60℃加热40 min,放冷30 min,扩散-吸收完毕后抽取进样瓶内溶液进行分析,安培检测器进行检测,以CN^(-)保留时间定性,以外标标准曲线法定量。氰化物(以CN^(-)计)检出限为0.5 ng/mL,且质量浓度在1~500 ng/mL范围内与色谱峰面积线性关系良好,相关系数大于0.99,加标回收率为71.3%~84.8%,测定结果的相对标准偏差均小于5%(n=6)。该方法简便、准确、灵敏度高,可用于血中氰化物的定性定量检验。A method for the determination of cyanide in blood by ion chromatography with diffusion-absorption extraction was established.1.0 mL blood sample was placed in a 10 mL headspace bottle and mixed with 1.0 mL ultrapure water.Then 0.5 mL of concentrated phosphoric acid was added and put into a 2.0 mL injection bottle containing 0.5 mL 0.25%NaOH solution.After sealing,the samples were heated at 60℃for 40 min and cooled for 30 min.After the diffusion-absorption was completed,the solution in the injection bottle was extracted for analysis,and the amperometric detector(AD)was used for detection.The CN^(−)retention time was used for qualitative analysis,and the external standard standard curve method was used for quantitative analysis.The detection limit of cyanide(CN^(−))was 0.5 ng/mL,and the mass concentration had a good linear relationship with the chromatographic peak area in the range of 1-500 ng/mL,the correlation coefficient was more than 0.99,and the extraction recovery were 71.3%-84.8%,and the relative standard deviations of the determination results were less than 5%(n=6).The method is simple,accurate and sensitive,and can be used for the qualitative and quantitative detection of cyanide in blood.

关 键 词：法医毒物学 氰化物 离子色谱 安培检测器 扩散-吸收 

分 类 号：O657.7[理学—分析化学]