摘要
采用液相色谱-串联质谱法测定血中毒芹碱、金雀花碱、秋水仙碱和α-茄碱等4种食源性植物毒素的含量。0.2mL血样用0.8mL乙腈去除血红蛋白,离心后,上层清液经0.22μm有机系微孔滤膜过滤。以Hypurity C_(18)色谱柱为分离柱,0.2%(体积分数)乙酸溶液(含有5mmol·L^(-1)乙酸铵,pH为4.0)和甲醇(20+80)的混合液为流动相进行等度洗脱,串联质谱分析中采用全扫描和选择反应监测模式。4种食源性植物毒素的质量浓度均在5.0～500μg·L^(-1)内与其对应的峰面积呈线性关系,检出限(3S/N)均为2.0μg·L^(-1),测定下限(10S/N)均为5.0μg·L^(-1)。在50,200,500μg·L^(-1)等3个浓度水平进行加标回收试验,回收率为84.5%～111%,测定值的相对标准偏差(n=5)为1.5%～6.2%。
LC-MS/MS was applied to the determination of 4 food borne plant toxins, i.e. coniine, cytisine, colchicine and solanine alkaloids in blood. Hemoglobin in 0.2 mL of blood sample was removed with 0.8 mL of acetonitrile. After centrifugation, the supernatant was filtered on 0.22 μm organic microporous filter membrane. Hypurity C18 chromatographic column was used as stationary phase, and the mixture of 0.2% （φ） acetic acid solution （containing 5 mmol· L^-1 ammonium acetate, pH was 4.0） and methanol （20＋80） was used as mobile phase in isometric elution. The full scanning mode and the selected reaction monitoring mode were adopted in MS/ MS. Linear relationships between values of peak area and mass concentration of the 4 food borne plant toxins were kept in the same range of 5.0-500 μg · L^-1 , with the same detection limit （3S/N） of 2.0 μg · L^ -1 and the same lower limit of determination （10S/N） of 5.0 μg · L^-1. Tests for recovery were made by standard addition method at the concentration levels of 50, 200, 500 μg · L^-1 giving values of recovery and RSDs （n = 5） in the ranges of 84.5%-111% and 1.5%-6.2% respectively.
作者
张婷
刘亚峰
孙册
赵欣彤
ZHANG Ting1 , LIU Yafeng1 , SUN Ce2 , ZHAO Xintong1(1. Department of Forensic Chemistry, Criminal Investigation Police University of China , Shenyang 110035, China 2. Evidence Identification Center of Jilin Province Public Security Department, Changchun 130051, China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2018年第11期1299-1302,共4页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
2016年国家级大学生创新训练计划项目(201610175049)
