同位素标记的(13)C3-西玛津的合成及土壤中西玛津分析的超高效液相色谱-串联质谱联用同时测定方法的建立
Synthesis of Isotopically Labeled (13)C3-Simazine and Development of a Simultaneous UPLC-MS/MS Method for the Analysis of Simazine in Soil.
作者信息
Song Yan, Guo Yangzhen, Zhang Xia, Yang Yue, Chen Shuo, She Gaimei, She Dongmei
机构信息
Plant Protection Institute of the Chinese Academy of Agricultural Sciences, Beijing 100193, China.
College of Pharmacology, Ningxia Medical University, Yinchuan 750004, China.
出版信息
Molecules. 2016 Jan 14;21(1):89. doi: 10.3390/molecules21010089.
The isotope dilution mass spectrometry (IDMS) is a highly efficient method for tackling the ion suppression in complex matrix by ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS), but a lack of commercial internal standards is a limiting factor for these analyses. Herein, an economical and efficient strategy for the synthesis of (13)C3-simazine via a three-step procedure was developed. The isotope-labeled internal standard was used for determination of simazine residue in soil samples. The quantitation method has a limit of detection of 0.015 μg/kg and quantitation of 0.08 μg/kg. The inter-day and intra-day precision of the method were below 4.6%. Recovery values were ranged between 92.9% and 99.2%. All the samples obtained from six provinces in China contained from 1 to 62 μg/kg of simazine.
同位素稀释质谱法（IDMS）是一种通过超高效液相色谱-串联质谱法（UPLC-MS/MS）解决复杂基质中离子抑制问题的高效方法，但缺乏商业内标是这些分析的一个限制因素。在此，开发了一种通过三步法合成(13)C3-西玛津的经济高效策略。该同位素标记内标用于测定土壤样品中的西玛津残留。该定量方法的检测限为0.015μg/kg，定量限为0.08μg/kg。该方法的日间和日内精密度均低于4.6%。回收率在92.9%至99.2%之间。从中国六个省份采集的所有样品中，西玛津含量为1至62μg/kg。
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