Method for determining bensulfuron methyl in water by boron trifluoride derivation-gaschromatographic mass spectrometry method
A gas chromatography-mass spectrometry and boron trifluoride technology, which is applied in the field of analysis of benzpiriodine in water by boron trifluoride derivatization-gas chromatography-mass spectrometry, can solve the problem of high detection limit, poor qualitative accuracy, poor reproducibility, etc. problems, to achieve the effect of low analysis cost, low detection limit, and stable baseline
Inactive Publication Date: 2013-06-26
NORTHEAST INST OF GEOGRAPHY & AGRIECOLOGY C A S
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Problems solved by technology
At present, scholars at home and abroad have carried out a lot of research on the residue, enrichment and harm of BSM in various environmental media, but some researches have not obtained ideal research results due to the limitation of analytical methods. The determination of BSM in water is often carried out by liquid chromatography. , due to the complexity of organic components in natural water bodies, large interference, complex pretreatment process is required, the reproducibility is poor, the detection limit of the method is also high, and the qualitative accuracy is poor, "Bensulfuron-methyl in rice paddy soil and water The detection limit of BSM in water reported in "Residue Analysis Method" is only 10ng / L
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Embodiment 1
[0019] A kind of boron trifluoride derivation provided by the present invention-gas chromatography mass spectrometry is analyzed the method for benziridone in water, concrete steps are as follows:
[0020] (1) Sampling: Take 1L of the water sample to be tested and place it in a conical flask;
[0021] (2) Preparation of standard addition solution: Take another 1L of distilled water, add 1mL of standard solution with a concentration of 1μg / mL, and place it in a conical flask;
[0022] (3) The first liquid-liquid extraction: Add 50 mL of dichloromethane to the solutions of (1) and (2) conical flasks respectively, shake for 1 minute, let stand to separate layers, and collect the dichloromethane phases in 2 According to the above extraction steps, extract 2 more times, combine and collect the extracted dichloromethane phases of (1) and (2) solutions respectively, and concentrate the dichloromethane phases to dryness by rotary evaporation;
[0023] (4) Add 1mL of methanol and 0.2m...
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The invention provides a method for determining bensulfuron methyl in water by a boron trifluoride derivation-gaschromatographic mass spectrometry method, which is applicable to analyzing the bensulfuron methyl in various water bodies. The method takes the BF3 as a derivation agent to accelerate the bensulfuron methyl to react to generate a derived organic matter with a lower boiling point, which is suitable for gaschromatographic mass spectrometry analysis; and then the gaschromatographic mass spectrometry is used for analyzing the derived organic matter to determine the content of the bensulfuron methyl. According to the method disclosed by the invention, the influences on interference components in a sample can be reduced, a base line adjacent to a chromatographic peak of the bensulfuron methyl is stable and the inferences are smaller; 1L of a large-volume sample is extracted and then is concentrated and analyzed, so that the detection limitation of the method is very low and the sensitivity of derived products is higher; and therefore, the detection limitation of the bensulfuron methyl is lower, the detection limitation of the method is 0.1ng / L through calculation, needed materials and equipment are simple and the analyzing cost is low.
Description
[0001] technical field [0002] The invention relates to a method for analyzing the herbicide BSM (bensulfuron-methyl) in water samples, in particular to a method for analyzing bensulfuron-methyl in water by boron trifluoride derivation-gas chromatography mass spectrometry. Background technique [0003] BSM (benzsulfuron-methyl) is a common herbicide, suitable for controlling annual and perennial broad-leaved weeds and sedges in paddy fields, with a half-life of 143 days at a pH value of 7, and a longer half-life in alkaline water. The farmland recedes into rivers, lakes and other water bodies, causing certain harm to aquatic organisms (PAN Huiyun, LI Xiaolu, XU Xiaohua, GAO Shixiang. Phytotoxicity of four herbs on Ceratophyllum demersum, Vallisneria natans and Elodea nuttallii. Journal of Environmental Sciences, 2009, 21: 307–312). At present, scholars at home and abroad have carried out a lot of research on the residue, enrichment and harm of BSM in various environmental ...
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IPC IPC(8): G01N30/02
Inventor 王健王国平张玉霞
Owner NORTHEAST INST OF GEOGRAPHY & AGRIECOLOGY C A S