Agilent Technologies, Alameda Araguaia, 1142, CEP 06455-000 Barueri, SP, Brazil.
Departamento de Química Fundamental - Instituto de Química - Universidade de São Paulo, Av. Prof. Lineu Prestes, 748, CEP 05508-000 São Paulo - SP, Brazil.
Food Chem. 2015 May 15;175:82-4. doi: 10.1016/j.foodchem.2014.11.137. Epub 2014 Nov 28.
A capillary electrophoresis-tandem mass spectrometry (CE-MS/MS) method for the determination of halosulfuron-methyl (HSU) residue in samples of sugarcane juice and tomato is introduced and validated. The samples were submitted to a QuEChERS extraction procedure followed by electrophoretic separation in NH4HCO3 electrolyte (adjusted to pH 8.5) and detection by electrospray-tandem mass spectrometry. The total HSU migration took place in less than 3.5 min, and the detection was accomplished by monitoring three fragmentation processes of this anion: m/z 435-182, 139, and 83. The R(2) values for concentrations up to 100 ppb (μg kg(-1)) were, respectively, 0.992, 0.992, and 0.978. Recovery values for samples spiked at three concentration levels (10, 20 and 50 ppb) were in the range of 96-104% with standard deviation not greater than 5.0%. The limit of detection for HSU in sugarcane juice and tomato was 2 ppb for both samples.
介绍并验证了一种毛细管电泳-串联质谱(CE-MS/MS)法,用于测定甘蔗汁和番茄样品中氯磺隆-甲酯(HSU)的残留量。样品经 QuEChERS 提取程序处理,然后在 NH4HCO3 电解质(调至 pH8.5)中进行电泳分离,并通过电喷雾串联质谱进行检测。总 HSU 迁移时间不到 3.5 分钟,通过监测该阴离子的三个碎裂过程来完成检测:m/z 435-182、139 和 83。浓度高达 100 ppb(μg kg(-1)) 的 R(2) 值分别为 0.992、0.992 和 0.978。在三个浓度水平(10、20 和 50 ppb)下添加样品的回收率在 96-104%范围内,标准偏差不超过 5.0%。甘蔗汁和番茄中 HSU 的检测限均为 2 ppb。