摘要
本研究应用QuEchERS法提取净化血液中拟除虫菊酯类农药,拟建立13种拟除虫菊酯类农药在血液样本中的GC-MS/MS检测方法。血液样品采用乙酸乙酯萃取、无水MgSO_(4)盐析振荡离心后,取上清液并移入装有20 mg PSA、30 mg C18、15 mg GCB粉末的离心管中净化,氮吹复溶后,使用GC-MS/MS多重反应监测(MRM)模式对检材进行定性定量分析。结果表明,13中拟除虫菊酯类农药的血液样本均能通过GC-MS/MS技术进行检测,在5~500μg·L^(-1)范围内,相关系数(R 2)在0.9937~0.9993之间,检出限(LOD)和定量限(LOQ)分别在0.2~2μg·L^(-1)、0.5~2μg·L^(-1)之间,平均回收率为73.49%~108.09%,日内精密度为1.30%~10.31%,日间精密度为1.70%~10.80%。该方法操作简便、检出限低、结果可靠,适用于法庭科学中血液样品中拟除虫菊酯类农药的检测。
In this study,QuEchERS method was used to the extract and purify pyrethroids in blood,and GC-MS/MS detection method for 13 pyrethroids in blood samples was established.The blood samples were extracted by ethyl acetate and salted out by anhydrous MgSO_(4) for shaking centrifugation.The supernatant was taken and transferred to a centrifuge tube containing 20mgPSA,30mgC18 and 15mgGCB powder for purification.After nitrogen blowing,the samples were analyzed by GC-MS/MS multiple reaction monitoring(MRM)mode for qualitative and quantitative analysis.The results showed that 13 pyrethroid pesticide blood samples could be detected by GC-MS/MS technology.The linear relationship was good in the range of 5~500μg·L^(-1),and the correlation coefficient(R 2)was 0.9937~0.9993.The limits of detection(LOD)and quantitation(LOQ)were 0.2~2μg·L^(-1)and 0.5~2μg·L^(-1),respectively.The average recoveries were 73.49%~108.09%,inter-day and intra-day precision were 1.30%~10.31%and 1.70%~10.80%,respectively.The method has the advantages of simple operation,low detection limit and reliable results,and is suitable for the detection of pyrethroid pesticides in blood samples in forensic science.
作者
张鹤耀
国菲
贾振军
李鹏
ZHANG He-yao;GUO Fei;JIA Zhen-jun;LI Peng(People s Public Security University of China,Beijing 100038,China;Judicial appraisal Center of Zibo Public Security Bureau Organization-Company,Zibo 255022,China;Shanxi Medical University,Taiyuan 030001,China)
出处
《化学研究与应用》
CAS
CSCD
北大核心
2022年第9期2128-2134,共7页
Chemical Research and Application
基金
中国人民公安大学基本科研业务费项目(2021JKF104)资助。
