College of Pharmacy, Kyungsung University, Busan, 48434, Republic of Korea.
Department of Pharmaceutical Science and Technology, Kyungsung University, Busan, 48434, Republic of Korea.
Forensic Sci Int. 2019 Sep;302:109846. doi: 10.1016/j.forsciint.2019.06.004. Epub 2019 Jun 13.
Pyrethroids, organic compounds similar to natural pyrethrums, constitute the majority of insecticides. Pyrethroids are widely used around the world owing to their excellent selective toxicity to certain insects. In addition, they are easily found in daily life, accounting for most household pesticides. Owing to the easy access to pyrethroid insecticides, pyrethroid-related accidents and suicides have occurred yearly. For the first time, nine pyrethroids commonly used in South Korea and their seven major metabolites were simultaneously analyzed and validated in human plasma using liquid chromatography triple quadrupole mass spectrometry. Plasmas spiked with these pyrethroids and their metabolites were prepared and deproteinized via the addition of acetonitrile. This deproteinized supernatant was filtered and directly injected to ascertain the liquid chromatography-tandem mass spectrometry. For a sensitive and reproducible analysis, all the pyrethroid and metabolite analysis conditions for the multiple reaction monitoring mode were optimized in advance and employed. The validation parameters of the method, including the specificity, linearity, limit of detection, limit of quantification, accuracy, precision, recovery, matrix effect, and stability were also evaluated. The R value of linearity was greater than 0.997 for all the analytes, the accuracy ranged from 81.8% to 112.3%, the precision from 0% to 10.1%, and the recovery from 90.9% to 112.4%, depending on the analyte. The stability was 97.0% to 107.0% in fresh plasma and 97.6% to 107.7% in corrupt plasma. The results were satisfactory for all the validation parameters. Furthermore, authentic pyrethroid-poisoned samples were analyzed using this validation method, to determine the suitability; deltamethrin and its metabolites, cis-DBCA and 3-PBA, were successfully analyzed.
拟除虫菊酯是与天然除虫菊酯相似的有机化合物，构成了大多数杀虫剂。由于对某些昆虫具有优异的选择性毒性，拟除虫菊酯在世界范围内得到了广泛应用。此外，它们在日常生活中很容易找到，占大多数家用杀虫剂的比例。由于容易获得拟除虫菊酯杀虫剂，每年都会发生与拟除虫菊酯相关的事故和自杀事件。首次采用液相色谱三重四极杆质谱法同时分析和验证了韩国常用的九种拟除虫菊酯及其七种主要代谢物在人血浆中的情况。通过加入乙腈对含有所谓拟除虫菊酯和代谢物的血浆进行沉淀和蛋白处理。对沉淀的上清液进行过滤，直接注入以确定液相色谱-串联质谱。为了进行灵敏且可重现的分析，所有拟除虫菊酯和代谢物分析条件都在多重反应监测模式下进行了优化。还评估了该方法的验证参数，包括特异性、线性、检测限、定量限、准确度、精密度、回收率、基质效应和稳定性。所有分析物的线性 R 值均大于 0.997，准确度范围为 81.8%至 112.3%，精密度范围为 0%至 10.1%，回收率范围为 90.9%至 112.4%，具体取决于分析物。新鲜血浆中的稳定性为 97.0%至 107.0%，腐败血浆中的稳定性为 97.6%至 107.7%。所有验证参数的结果均令人满意。此外，还使用该验证方法分析了真实的拟除虫菊酯中毒样本，以确定其适用性；成功分析了氯菊酯及其代谢物顺式-DBCA 和 3-PBA。
