Ramesh Atmakuru, Ravi Perumal Elumalai
Department of Analytical Chemistry, Mass Spectrometry Division, International Institute of Biotechnology and Toxicology-IIBAT, Padappai, Chennai 601301, Tamil Nadu, India.
J Chromatogr B Analyt Technol Biomed Life Sci. 2004 Apr 5;802(2):371-6. doi: 10.1016/j.jchromb.2003.12.016.
A new rapid and sensitive electron ionization gas chromatography-mass spectrometry method in selective ion monitoring mode (SIM) was developed for the determination of l3 synthetic pyrethroid insecticide molecules and their stereo isomers in whole blood. The pyrethroid insecticides investigated are allethrin, bifenthrin, cypermethrin, cyphonothrin, cyfluthrin, lambda-cyhalothrin, deltamethrin, fenvalerate, fenpropathrin, imiprothrin, permethrin, prallethrin and transfluthrin. The residues of pyrethroids are extracted from the whole blood using hexane and acetone mixture (80 + 20%) as solvent. All the pyrethroid residues were separated by using a gas chromatography-mass spectrometry operated in electron ionization mode and quantified in selective ion monitoring mode. The method can detect the residues of different pyrethroids down to the level 0.05-2 ng/ml. Recovery experiments conducted in whole blood samples at the fortification level 1-1000 ng/ml showed 91-103% recovery. The applications of the analytical method for the determination of pyrethroid residues in real samples were tested by analyzing 45 human blood samples collected from the population exposed continuously to different pyrethroid based formulations. The results are confirmed by spiking the known quantity of pyrethroids and subsequently their positive detection.
建立了一种新的快速灵敏的电子电离气相色谱 - 质谱法,在选择性离子监测模式(SIM)下测定全血中13种合成拟除虫菊酯类杀虫剂分子及其立体异构体。所研究的拟除虫菊酯类杀虫剂有丙烯菊酯、联苯菊酯、氯氰菊酯、苯醚氰菊酯、氟氯氰菊酯、高效氯氟氰菊酯、溴氰菊酯、氰戊菊酯、甲氰菊酯、炔咪菊酯、氯菊酯、丙炔菊酯和四氟甲醚菊酯。以己烷和丙酮混合物(80 + 20%)为溶剂从全血中提取拟除虫菊酯类残留物。所有拟除虫菊酯类残留物通过电子电离模式操作的气相色谱 - 质谱仪进行分离,并在选择性离子监测模式下进行定量。该方法能够检测到低至0.05 - 2 ng/ml水平的不同拟除虫菊酯类残留物。在全血样品中进行的加标水平为1 - 1000 ng/ml的回收率实验显示回收率为91 - 103%。通过分析从持续接触不同拟除虫菊酯类制剂的人群中采集的45份人体血液样本,测试了该分析方法在实际样品中测定拟除虫菊酯类残留物的应用。通过添加已知量的拟除虫菊酯并随后进行阳性检测对结果进行了确认。