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为避免传统生物样本前处理的复杂过程,直接沉淀蛋白处理人体血液,在此基础上,采用场放大堆积在线富集技术检测人血中百草枯、敌草快和野燕麦3种季铵盐类除草剂。优化条件下,采用p H 4的200 mmol/L磷酸盐缓冲液(20%乙腈,V/V)为分离缓冲液,3.45 k Pa×3 s去离子水,10 k V电迁移进样30 s分析。其中百草枯和敌草快的检测限(LOD)为0.3μg/m L,野燕麦为0.8μg/m L;百草枯和敌草快线性范围为1~100μg/m L,野燕麦为2~100μg/m L,相关系数(r~2)均大于0.99。精密度(RSD)均小于7%。方法可用于该类农药中毒、死亡案件中血液样本的检测。
In order to avoid the complex process of traditional biological sample pretreatment, the protein was directly precipitated to treat human blood. On the basis of the above, three kinds of quaternary ammonium salts of paraquat, diquat and wild oat herbicide. Under optimized conditions, 200 μL phosphate buffer (20% acetonitrile, V / V) of p H 4 was used as the separation buffer and 3.45 kPa × 3 s deionized water. Electrokinetic injection of 10 k V was performed for 30 s analysis. The limit of detection (LOD) of paraquat and diquat was 0.3μg / m L and that of wild oats was 0.8μg / m L. The linear range of paraquat and diquat was 1 ~ 100μg / m L and that of wild oat was 2 ~ 100μg / m L, the correlation coefficient (r ~ 2) were greater than 0.99. Precision (RSD) are less than 7%. The method can be used for the detection of blood samples in such pesticide poisoning and death cases.