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法医学杂志 2018, Vol. 34 Issue (1) :37-43    DOI: 10.3969/j.issn.1004-5619.2018.01.008
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林  琳1,2,张素静1,徐渭聪1,3,骆如欣1,马  栋1,沈  敏1
1. 司法鉴定科学研究院 上海市法医学重点实验室 上海市司法鉴定专业技术服务平台,上海 200063; 2. 华东政法大学刑事司法学院,上海 200042; 3. 南方医科大学公共卫生学院,广东 广州 510515
Analysis of Arsenic Compounds in Blood and Urine by HPLC-ICP-MS
LIN Lin1,2, ZHANG Su-jing1, XU Wei-cong1,3, LUO Ru-xin1, MA Dong1, SHEN Min1
1. Shanghai Key Laboratory of Forensic Medicine, Shanghai Forensic Service Platform, Academy of Forensic Science, Shanghai 200063, China; 2. College of Criminal and Justice, East China University of Political Science and Law, Shanghai 200042, China; 3. School of Public Health, Southern Medical University, Guangzhou 510515, China

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摘要 目的 建立血液和尿液中6种砷形态化合物[AsC、AsB、As(Ⅲ)、DMA、MMA、As(Ⅴ)]的高效液相色谱-电感耦合等离子体质谱(high-performance liquid chromatography-inductively coupled plasma-mass spectrometry,HPLC-ICP-MS)分析方法,并应用于实际案例。 方法 利用曲拉通破坏细胞,以乙二胺四乙酸二钠盐二水合物络合细胞内砷形态化合物,超声水浴加乙腈沉淀蛋白进行样品前处理,采用Hamilton PRP-X100阴离子分析柱,碳酸铵水溶液与超纯水作为流动相,对样品中砷形态化合物进行梯度洗脱后,采用ICP-MS分析样品中砷形态化合物。 结果 血液中砷形态化合物检测限为1.66~10 ng/mL,最低定量限为5~30 ng/mL,尿液中砷形态化合物检测限为0.5~10 ng/mL,最低定量限为5~30 ng/mL,日内、日间精密度的相对标准偏差不超过10%,且成功应用于3组案例。 结论 本研究建立了血液和尿液中常见6种砷形态化合物的分析方法,该方法适用于涉砷中毒案件的司法鉴定及砷剂治疗患者血液和尿液中砷形态化合物的检测。
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关键词法医毒理学   高效液相色谱-电感耦合等离子体质谱   砷剂   血液   尿     
Abstract: Objective To establish an analysis method for the detection of 6 arsenic compounds [AsC, AsB, As(Ⅲ), DMA, MMA and As(V)] in blood and urine by high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS), and apply it to real cases. Methods Triton was used to damage cells, and then EDTA·2Na·2H2O was used to complex arsenic compounds in cells, and sonication and protein deposition by acetonitrile were performed for sample pretreatment. With the mobile phase consisted of ammonium carbonate and ultrapure water, gradient elution was performed for obtaining the arsenic compounds in samples, which were analysed by ICP-MS with Hamilton PRP-X100 column. Results The limits of detection in blood were 1.66-10 ng/mL, while the lower limits of quantitation in blood ranged from 5 to 30 ng/mL. The limits of detection in urine were 0.5-10 ng/mL, while the lower limits of quantitation in urine were 5-30 ng/mL. The relative standard deviation of inter-day and intra-day precisions was less than 10%. This method had been successfully applied to 3 cases. Conclusion This study has established an analysis method for detecting 6 common arsenic compounds in blood and urine, which can be used to detect the arsenic compounds in the blood and urine from arsenic poisoning cases as well as the patients under arsenic treatment.
Keywordsforensic toxicology   high-performance liquid chromatography-inductively coupled plasma-mass spectrometry (HPLC-ICP-MS)   arsenicals   blood   urine     

“十三五”国家重点研发计划资助项目(2016YFC0800 704,2016YFC0503607);国家自然科学基金资助项目(81671868, 81302613);上海市科学技术委员会资助项目(15dz1207500);上海市法医学重点实验室资助项目(17DZ2273200);上海市司法鉴定专业技术服务平台资助项目(16DZ2290900)

Corresponding Authors: 沈敏,女,研究员,主要从事毒物分析研究;E-mail:shenm@ssfjd.cn 马栋,男,副研究员,主要从事毒物分析研究;E-mail:modong@ssfjd.cn   
About author: 林琳(1991—),女,硕士研究生,主要从事毒物分析研究;E-mail:idea00@yeah.net
林琳, 张素静, 徐渭聪,等.血液和尿液中砷形态化合物的HPLC-ICP-MS分析[J]  法医学杂志, 2018,34(1): 37-43
LIN Lin, ZHANG Su-Jing, XU Wei-Cong,et al..Analysis of Arsenic Compounds in Blood and Urine by HPLC-ICP-MS[J]  , 2018,34(1): 37-43
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