Citation: LI Gui-Jie, WANG Da-Wei, DING Lan. Rapid Extraction of Triazine Herbicides in Cereal by Microwave-assisted Steam Extraction Combined with Solidification of Floating Organic Drop Method[J]. Chinese Journal of Analytical Chemistry, ;2018, 46(12): 2011-2018. doi: 10.11895/j.issn.0253-3820.181199 shu

Rapid Extraction of Triazine Herbicides in Cereal by Microwave-assisted Steam Extraction Combined with Solidification of Floating Organic Drop Method

LI Gui-Jie ^1,2, ,
WANG Da-Wei ¹ ,
DING Lan ²

1.
College of Food Science, Jilin Agricultural University, Changchun 130033, China;
2.
College of Chemistry, Jilin University, Changchun 130012, China

Received Date: 24 March 2018
Revised Date: 4 September 2018

Fund Project: This work was supported by the National High Technology Research and Development Program of China (No. 2011AA100805-1) and the Major Project for Science and Technology Development of Jilin Province, China (No. 2012ZDGG007).

A simple sensitive and green method was established for the rapid determination of six kinds of triazine herbicides in cereal samples. The method combined the advantages of microwave assisted extraction, water steam extraction and floating solvent extraction. Certain amount of dodecanol was added to the sample in the extraction vessel, and then triazines were extracted by water steam under microwave energy, after that, sodium chloride was added into the extract liquor. After the extract liquor was thoroughly stirred and put into the ice-water bath, the sample scoop was taken out and the dodecanol solid of triazine herbicide was removed and transferred to the centrifuge tube. After thawing, the content was filtered, and then triazine herbicides were tested by liquid chromatography tandem mass spectrometry. In the experiment, the experimental conditions of microwave assisted water steam extraction and solidification of floating organic drop were optimized. Under the optimal experimental conditions such as 800 W of microwave extraction power, 12 mL of extract liquor volume, 140 μL of dodecanol as floating solvent, 2.0 g of NaCl and extract liquior at pH 7, the linearity region for detection of six triazine herbicides was 2-200 ng/g, with correlation coefficient of 0.9979-0.9998. The limits of detection and the recoveries of triazines were 0.28-0.61 ng/g and 82.2%-99.5%, respectively. The relative standard deviations of intra-day and inter-day variations were 2%-7% and 3%-6%, respectively. Compared with the traditional extraction method, the proposed method was more environmentally friendly, rapid in detection and simpler in operation. Besides, the method had many advantages such as low cost, high concentration fold and low organic solvent, and could be used for detection of triazine herbicides in complex solid samples.
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