文章建立了一种QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)前处理结合气相色谱-串联质谱(Gas chromatography-tandem mass spectrometry,GC-MS/MS)检测刺梨中28种有机氯和拟除虫菊酯农药残留的方法。样品经乙腈提取,N-丙基...文章建立了一种QuEChERS(Quick,Easy,Cheap,Effective,Rugged and Safe)前处理结合气相色谱-串联质谱(Gas chromatography-tandem mass spectrometry,GC-MS/MS)检测刺梨中28种有机氯和拟除虫菊酯农药残留的方法。样品经乙腈提取,N-丙基乙二胺(Primary secondary amine,PSA)和十八烷基键合硅胶(C18)粉末分散固相萃取净化浓缩后,采用GC-MS/MS选择反应监测模式(Selected reaction monitoring,SRM)测定,外标法定量。结果表明:28种农药在10~500μg/L的浓度范围内,各农药峰面积与进样质量浓度间线性关系良好,决定系数(R^(2))>0.9959,定量限低于0.0042 mg/kg;在添加水平分别为0.005、0.05及0.25 mg/kg时,28种农药的平均回收率为81.4%~107.1%,相对标准偏差为1.07%~9.44%。该方法能够有效消除基质效应的影响,实现对刺梨中28种农药的残留进行快速准确的测定。展开更多
Molecular fluorescence spectrometry, resonance Rayleigh scattering and gas chromatography-mass spectroscopy（GC-MS） were used to study the effect of pure fish serum albumin（FSA） as the model protein on the extracti...Molecular fluorescence spectrometry, resonance Rayleigh scattering and gas chromatography-mass spectroscopy（GC-MS） were used to study the effect of pure fish serum albumin（FSA） as the model protein on the extraction of three chlorobenzenes（CBs： 1,3-DCB, 1,2-DCB and 1,2,4-TCB; DCB=dichlorobenzene; TCB=trichlorobenzene） in fish samples. The results show that there was a strong binding effect between CB and FSA. In an aqueous solution of 90%（volume fraction） acetone, a slow but full protein denaturation might take place, which would cause the unfolding of protein and the releasing of CBs. Based on these results, a QuEChERS（quick, easy, cheap, effective, rugged and safe） method was modified by replacing the traditional acetonitrile with acetone aqueous solution in the present work. This modified QuEChERS method was applied in the determination of CBs in fish samples. The spiked recoveries and the limits of detection were 80.4%--118.3% and 2.4--7.3 ng/g, respectively. This paper proposes a new strategy by slowing down the protein denaturation and releasing bound organic compounds to enhance the extraction efficiency of CBs in fish samples.展开更多
基金Natural Science Foundation of Shandong Province,China
文摘Molecular fluorescence spectrometry, resonance Rayleigh scattering and gas chromatography-mass spectroscopy（GC-MS） were used to study the effect of pure fish serum albumin（FSA） as the model protein on the extraction of three chlorobenzenes（CBs： 1,3-DCB, 1,2-DCB and 1,2,4-TCB; DCB=dichlorobenzene; TCB=trichlorobenzene） in fish samples. The results show that there was a strong binding effect between CB and FSA. In an aqueous solution of 90%（volume fraction） acetone, a slow but full protein denaturation might take place, which would cause the unfolding of protein and the releasing of CBs. Based on these results, a QuEChERS（quick, easy, cheap, effective, rugged and safe） method was modified by replacing the traditional acetonitrile with acetone aqueous solution in the present work. This modified QuEChERS method was applied in the determination of CBs in fish samples. The spiked recoveries and the limits of detection were 80.4%--118.3% and 2.4--7.3 ng/g, respectively. This paper proposes a new strategy by slowing down the protein denaturation and releasing bound organic compounds to enhance the extraction efficiency of CBs in fish samples.
