摘要
目的建立一种快速检测琥珀胆碱的方法。方法血液样品经过乙腈沉淀蛋白后,以0.22μm滤膜过滤,利用高效液相色谱-飞行时间质谱联用仪检测毒狗针及狗血中琥珀胆碱成分。选用Kinetex 2.6μm HILIC（100mm×2.1 mm）并前接保护柱,以5 mmol醋酸铵90%乙腈水溶液和200 mmol醋酸铵0.4%甲酸水溶液作为流动相,进行等度洗脱分离。结果前处理简单快速,检测时间仅需5 min。采用的定性定量离子其精确分子量为145.109 3Da。测得血液样品中琥珀胆碱的检测限为0.9 ng/m L（S/N=10）,方法的线性范围为0.01~10μg/m L。结论该方法准确可靠、简便快速,具有良好重现性,是琥珀胆碱的一种有效检测方法。
Objective Succinylcholine, a short-acting agent to depolarize skeletal muscle, is currently used in anesthesia for its fast activation, being frequently chosen to poison dogs by culprits making their hitting darts daubed with it. Therefore, its residues in dog body will be harmful for the people who eat the dog meat. This paper aimed at establishing methods for the detection of succinylcholine in biological samples. Methods Aliquots of 2 m L human blood samples containing succinylcholine were prepared for analysis. Succinylcholine was extracted from human plasma with only two steps by acetonitrile to precipitate protein and the 0.22 μm filtering membrane to conduct filtration. The samples were separated by high performance liquid chromatography through a Kinetex 2.6 μm HILIC（100 mm×2.1 mm） column of Shimadzu 30 A. The liquid chromatography-mass spectrometry was carried out by selection of isocratic elution, salinity and acidity of mobile phase together with the optimization of mass spectrometry. The mobile phases were consisted of acetonitrile（diluted to 90 % with the buffer of 5 mmol/L ammonium acetate, designated as A） and 200 mmol ammonium acetate/0.4% formic acid（B）, running at the flow rate of 0.5 m L/min. Results The detection was completed within 5 min, the precise molecular weight of ion selected for qualitative and quantitative was 145.1093 Da. By stepwise dilution, the measured quantitative detection limit was 0.9 ng/m L（S/N=10） in blood, and the linear range was from 0.01 to 10 μg/m L. Conclusions This method is accurate, reliable, simple, rapid and repeatable, and can be applied to the forensic toxicological analysis.
出处
《刑事技术》
2016年第2期120-122,共3页
Forensic Science and Technology
