适用于法庭科学毒物分析的干血斑检验体系的建立——以5种常见药(毒)物为例  

Development of an analytical system for dried blood spots for forensic toxicology:a case study of five common drugs and poisons

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作  者:苏东斌 董林沛 张云峰 赵鹏 李开开[1] SU Dongbin;DONG Linpei;ZHANG Yunfeng;ZHAO Peng;LI Kaikai*(College of Investigation,People’s Public Security University of China,Beijing 100038,China;Institute of Forensic Science,Ministry of Public Security,Beijing 100038,China)

机构地区:[1]中国人民公安大学侦查学院,北京100038 [2]公安部鉴定中心,北京100038

出  处:《色谱》2024年第3期245-255,共11页Chinese Journal of Chromatography

基  金:公安部技术研究计划(2022JSYJC008)。

摘  要:干血斑技术能够方便地对血液样品中的违禁药物进行快速分析,在酒后驾驶检查、滥用药物检测、兴奋剂检测等毒物分析场景具有显著优势。然而在我国法庭科学毒物分析领域,因缺少标准化检验体系,其稳定性和可靠性未得到深入研究论证,限制了其在司法实践中的运用。本研究以甲基苯丙胺、利多卡因、氯胺酮、芬太尼和地西泮为典型药(毒)物,使用整个干血斑进行分析,建立了适用于法庭科学领域毒物分析的超高效液相色谱-串联质谱分析方法,形成了以干血斑样品制作、前处理、分析、储存和效用性评价为主要内容的检验体系,并为干血斑中其他药(毒)物的分析方法开发提供参考。结果表明,干血斑中利多卡因和芬太尼在0.5~100 ng/mL内线性关系良好,甲基苯丙胺、氯胺酮、地西泮在2~100 ng/mL内线性关系良好,方法检出限为0.2~0.5 ng/mL。干血斑中5种目标物可以在60天内保持稳定,目标物测定含量与理论值的偏差在15%以内。干血斑中5种目标物的测量结果与全血一致,没有显著的系统误差和比例误差,芬太尼、地西泮、氯胺酮、利多卡因和甲基苯丙胺的测量浓度的相对偏差分别为4.44%、3.50%、7.66%、5.10%和5.25%。干血斑样品前处理方法简单,样品用量小,能够实现血液样品保存的轻量化和规范化且与全血样品具有高度定量一致性,可为公安实践工作中分析、保存血液检材提供新方案。Dried blood spot(DBS)technology is a simple and convenient method for collecting,transporting,and storing blood samples on filter paper,and has numerous applications in the clinical,research,and public health settings.This technique is gaining popularity in the field of forensic science because it facilitates the rapid analysis of prohibited drugs in blood samples and offers significant advantages in toxicology scenarios such as drinking-driving screening,drug abuse detection,and doping detection.However,the lack of a standardized system and the fact that its stability and reliability have not been thoroughly researched and demonstrated limit its application in judicial practice in China.DBS samples can be prepared,stored,and analyzed in various ways,all of which may significantly affect the results.In this study,we developed a method based on ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)that focuses on the preparation,pretreatment,analysis,and storage of DBS samples.A thorough investigation was conducted to examine the optimal preparation conditions,including the blood spot matrix,drying technique,and preprocessing parameters,such as the solvent and extraction method.Moreover,the analytical conditions,such as the mobile phase system and elution gradient,were established to facilitate the quantitative detection of methamphetamine,lidocaine,ketamine,fentanyl,and diazepam in both DBS and whole-blood samples.The impact of storage conditions,such as the temperature,humidity,and sealing,on the analytical results of the DBS and whole-blood samples was also examined.The results showed a strong linear relationship for lidocaine and fentanyl within the range of 0.5-100 ng/mL.Similarly,methamphetamine,ketamine,and diazepam exhibited good linearity within the range of 2-100 ng/mL.The coefficients of determination(r 2)ranged from 0.9983 to 0.9997,and the limits of detection ranged from 0.2 to 0.5 ng/mL,indicating a high degree of correlation and sensitivity.Stability tests demonstrated th

关 键 词:超高效液相色谱-串联质谱 毒物分析 干血斑 储存条件 稳定性 

分 类 号:O658[理学—分析化学]

 

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