Simultaneous determination of amitraz, chlordimeform, formetanate and their main metabolites in human urine by high performance liquid chromatography-tandem mass spectrometry
Simultaneous determination of amitraz, chlordimeform, formetanate and their main metabolites in human urine by high performance liquid chromatography-tandem mass spectrometry
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DOI：
10.1016/j.jchromb.2017.03.004
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发表时间：
2017-05-01
影响因子：
3
通讯作者：
Guo, Hao
中科院分区：
文献类型：
--
作者：
Gao, Xue;Tan, Yanglan;Guo, Hao
建立了一种快速、简便、可靠的高效液相色谱-串联质谱（HPLC-MS/MS）法同时测定人尿中双甲脒、杀虫脒、甲氰菊酯及其主要代谢物N-（2，4-二甲基苯基）-N-甲基甲脒（DMPF）、2，4-二甲基甲脒（DMF）、2，4-二甲基苯胺（DMA）、4-氯-2-甲基苯胺和3-羟基乙酰苯胺的方法。将尿样与缓冲溶液（pH 8）混合，随后通过固载液/液萃取（SLE）净化。采用沃茨Atlantis T3色谱柱（150 mm × 4.6 mm，5 μ m）分离，电喷雾离子源正离子化，串联质谱多反应监测（MRM）模式定量。为了尽量减少基质效应，采用了8种分析物的基质匹配校准曲线，相关系数（R-2）大于0.99。通过测定检测限（LOD，0.3-0.6 ng/mL）、定量限（LOQ，1.0-2.0 ng/mL）和回收率（89.1%-108.4%）以及日内和日间相对标准偏差（RSD，
A rapid, simple and reliable high performance liquid chromatography -tandem mass spectrometry (HPLC MS/MS) method was developed for simultaneous determination of amitraz, chlordimeform, formetanate and their main metabolites, N-(2,4-dimethylphenyl)-N-methyl-formamidine (DMPF), 2,4-dimethylformamidine (DMF), 2,4-dimethylaniline (DMA), 4-chloro-2-methylaniline and 3hydroxyacetanilide in human urine. The urine samples were mixed with buffer solutions (pH 8) and subsequently cleaned up by solid supported liquid/liquid extraction (SLE). The target analytes were efficiently separated with a Waters Atlantis T3 column (150 mm x 4.6 mm, 5 mu m), ionized with electrospray ion source in positive mode, and quantitatively determined by tandem mass spectrometry in the multiple reaction monitoring (MRM) mode. In order to minimize matrix effects, the matrix -matched calibration curves of eight analytes were adopted with correlation coefficients (R-2) above 0.99. The method were further validated by determining the limits of detection (LODs, 0.3-0.6 ng/mL), the limits of quantitation (LOQs, 1.0-2.0 ng/mL) and recoveries (89.1%-108.4%) with intra-day and inter -day relative standard deviation (RSD,