LC-MS/MS (liquid chromatography-mass spectrometry/mass spectrometry) method for analyzing residual quantity of phenoxy carboxylic acid herbicides in tobaccos
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A phenoxycarboxylic acid and LC-MS technology, which is applied to the analysis of materials, measurement devices, and material separation, can solve the problems of underestimating the actual concentration, etc., and achieve the effects of reducing matrix effects, improving accuracy, and operating accurately
Active Publication Date: 2014-04-02
CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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Ordinary pretreatment methods mostly directly use acidifying reagents to extract target compounds, and phenoxycarboxylic acid herbicides usually exist in the form of free acids, salts, or esters, and the detection of only acidifying reagents will eventually underestimate their actual concentration
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example 1
[0037] 1. Instruments and reagents:
[0038] Standards of 2,4,5-T, 2,4-D, dicamba and their methyl ester derivatives were purchased from Dr. Eh laboratory in Germany; deuterated 2,4,5-T, deuterated 2,4- D and deuterated dicamba standard products were purchased from Canadian CDN company.
[0039] Methanol (Pesticide Residue Grade, DUKSAN Company, South Korea); Dichloromethane (Pesticide Residue Grade, J. T. Baker Company, USA); Glacial Acetic Acid (HPLC Grade, TEDIA Company, USA); C18 (Agilent Company, USA); Anhydrous Magnesium Sulfate (Tianjin Kemiou Chemical Reagent Co., Ltd.), should be burned at 650 ℃ for 4 h before use, and stored in a desiccator for later use; sodium hydroxide (Tianjin Chemical Reagent No. 3 Factory); concentrated sulfuric acid (Luoyang Haohua Chemical Reagent Co., Ltd.) .
[0040] Liquid chromatography-tandem mass spectrometry (API 4000, American AB Company); desktop high-speed refrigerated centrifuge (3-30k, American SIGMA Company); vortex oscillator...
example 2
[0057] As described in Example 1, another tobacco sample B was selected, and the measured contents of the three pesticide targets in the sample are shown in Table 4.
[0058] Table 4 Detection results of pesticide targets in sample B
[0059] serial number Chinese common name Content of pesticide target in the sample (mg / kg) 1 2,4,5-T 0.16 2 2,4-D not detected 3 Dicamba not detected
example 3
[0061] As described in Example 1, another tobacco sample C was selected, and the measured contents of the three pesticide targets in the sample are shown in Table 5.
[0062] table 5 Detection results of pesticide targets in sample C
[0063] serial number Chinese common name Content of pesticide target in the sample (mg / kg) 1 2,4,5-T not detected 2 2,4-D 0.34 3 Dicamba not detected
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Abstract
The invention relates to an LC-MS / MS (liquid chromatography-mass spectrometry / mass spectrometry) method for analyzing residual quantity of phenoxy carboxylic acid herbicides in tobaccos. The LC-MS / MS method is characterized by carrying out analysis and determination through the following steps: wetting and hydrolyzing a sample through a NaOH solution, then acidifying with H2SO4, adding methylene dichloride and an internal standard substance, carrying out vortex extraction, dewatering an extracting solution with anhydrous MgSO4, purifying with C18, and taking and determining supernate by adopting an LC-MS method. Through the method, an existing sample treatment method is improved, the cleaner supernate solution is provided, and the maintenance quantity of an instrument in the usage process can be reduced. Compared with the prior art, the LC-MS / MS method has the following excellent effect that the hydrolysis purpose while wetting is achieved by changing 'wetting the sample with water' into 'wetting the sample with the NaOH water solution'. By adding the H2SO4 solution to regulate PH value, all the phenoxy carboxylates and esters can be converted into free acids which can be detected, and the detection accuracy can be improved. Compared with acetonitrile extraction, the methylene dichloride selected as an extractant has better pertinence, and the extraction effect can be enhanced.
Description
technical field [0001] The invention belongs to the technical field of pesticide residue detection in tobacco, and in particular relates to an LC-MS / MS method for analyzing the residual amount of three phenoxycarboxylic acid herbicides in tobacco. NaOH solution is added to tobacco samples and hydrolyzed by lye The process converts all phenoxycarboxylic acid herbicides in different forms such as acid, salt and ester into the form of salt, and then converts them all into free acid form by adjusting the pH value with sulfuric acid, and then extracts with dichloromethane, C18 Sorbent purification and determination by liquid chromatography-tandem mass spectrometry (LC-MS / MS). Background technique [0002] Phenoxycarboxylic acid herbicides are by far the second largest selective herbicides in the world, and also the largest herbicides against broadleaf weeds in the world. Phenoxycarboxylic acid herbicides belong to low-toxic herbicides, but they have endocrine disrupting effects....
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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 刘珊珊边照阳杨飞李中皓范子彦张洪非王颖张艳革唐纲岭胡清源
Owner CHINA NAT TOBACCO QUALITY SUPERVISION & TEST CENT
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