Chamkasem Narong
a Southeast Food and Feed Laboratory (SFFL), U.S. Food and Drug Administration , Atlanta , Georgia , USA.
J Environ Sci Health B. 2018;53(9):622-631. doi: 10.1080/03601234.2018.1473977. Epub 2018 May 22.
A simple high-throughput liquid chromatography/tandem mass spectrometry (LC-MS/MS) multiresidue analysis method was developed for the simultaneous determination of polar pesticides, plant growth regulators and other polar compounds. These included amitrole, chlormequat, mepiquat, cyromazine, ETU, PTU, perchlorate, and daminozide using a mixed-mode column. A 10 g test portion was shaken with acidified methanol for 10 min. After centrifugation, the sample extract was injected and analyzed within 11 min by LC-MS-MS. This column eliminated the need for derivatization or the use of ion paring reagent. Two MS-MS transitions were monitored in the method for each target compound to achieve true positive identification. Eight isotopically-labeled internal standards corresponding to each analyte were used to correct for matrix suppression effect and/or instrument signal drift. The average recovery for all analytes at 20, 40, and 250 ng/g (n = 6) ranged from 73-136%, with a relative standard deviation of ≤ 20%.
开发了一种简单的高通量液相色谱/串联质谱(LC-MS/MS)多残留分析方法,用于同时测定极性农药、植物生长调节剂和其他极性化合物。这些化合物包括杀草强、矮壮素、甲哌鎓、环丙氨嗪、乙撑硫脲、丙硫脲、高氯酸盐和氨基脲,使用混合模式柱进行分析。称取10 g试样,与酸化甲醇振荡10分钟。离心后,将样品提取物注入LC-MS-MS中,并在11分钟内完成分析。该色谱柱无需衍生化或使用离子对试剂。该方法中对每种目标化合物监测两个MS-MS跃迁,以实现真正的阳性鉴定。使用与每种分析物对应的八种同位素标记内标来校正基质抑制效应和/或仪器信号漂移。所有分析物在20、40和250 ng/g(n = 6)水平下的平均回收率为73-136%,相对标准偏差≤20%。