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CN-119901838-B - Determination method and application of enazachlor, florasulam and/or triazoxamide in feed

CN119901838BCN 119901838 BCN119901838 BCN 119901838BCN-119901838-B

Abstract

The invention discloses a method for measuring novel herbicide of clethodim, florasulam and/or triazoxamide in feed and application thereof. Belongs to the technical field of pesticide residue detection. The invention provides a method for determining novel herbicides of clethodim, florasulam and triazoxamide in feed, which is based on a dispersion solid phase extraction pretreatment technology, does not need a solid phase extraction column, has low cost of reagents used, realizes effective purification and enrichment of three novel herbicides, and can quickly and accurately determine whether the animal feed contains the herbicides of florasulam, clethodim, triazoxamide and the like and corresponding residual quantity by combining ultra-high performance liquid chromatography tandem mass spectrometry UPLC-MS/MS.

Inventors

  • XUE KANG
  • HU JIANGTAO
  • GONG TINGTING
  • CHENG TIEYUAN
  • ZHENG TINGTING
  • WANG XIXI
  • LIU JUN

Assignees

  • 成都海关技术中心

Dates

Publication Date
20260508
Application Date
20250120

Claims (5)

  1. 1. The method for determining the enazachlor, the florasulam and/or the triazoxamide in the feed is characterized by comprising the following steps of: (1) Sample pretreatment, namely taking a sample to be detected, adding water, uniformly mixing, standing for 15-30min, adding an extraction solvent and a homogenizer, and shaking uniformly to obtain a primary extract; (2) Adsorption of impurities and water, namely adding an adsorbent into the primary extract, vibrating at high speed, centrifuging, and taking supernatant to obtain a secondary extract; (3) Purifying the extracting solution, namely adding a purifying reagent into the second-stage extracting solution, performing vortex vibration treatment, centrifuging, taking supernatant, and filtering to obtain a solution to be detected; (4) High performance liquid chromatography tandem mass spectrometry detection, namely, introducing detection liquid into the high performance liquid chromatography tandem mass spectrometry for qualitative and quantitative detection; the extraction solvent in the step (1) is acetic acid-acetonitrile solution with the concentration of 1%, and the addition amount is 15mL/5g of sample to be detected; The adsorbents in the step (2) are anhydrous magnesium sulfate and sodium acetate, and the addition amounts are 6.0g/5g of sample to be detected and 1.5g/5g of sample to be detected respectively; The purifying reagent in the step (3) is anhydrous magnesium sulfate, C 18 and PSA, and the adding amount is 150mg/mL of secondary extracting solution, 50mg/mL of secondary extracting solution and 50mg/mL of secondary extracting solution respectively; The chromatographic conditions of the high performance liquid chromatography in the step (4) are as follows: a chromatographic column ACQUITY UPLC HSS T, 1.8 μm, 2.1X100 mm; the mobile phase is 0.1% formic acid aqueous solution of phase A, and acetonitrile solution of phase B; Elution-gradient elution, elution procedure is as follows: 0-0.5min, the dosage of mobile phase A is 50%, and the dosage of mobile phase B is 50%; 0.5-4min, the consumption of the mobile phase A is gradually decreased from 50% to 20% at a constant speed, and the consumption of the mobile phase B is gradually increased from 50% to 80% at a constant speed; 4-5min, the dosage of the mobile phase A is 20%, and the dosage of the mobile phase B is 80%; 5-5.5min, increasing the dosage of the mobile phase A from 20% to 50% at uniform speed, and decreasing the dosage of the mobile phase B from 80% to 50% at uniform speed; 5.5-7min, the dosage of the mobile phase A is 50%, and the dosage of the mobile phase B is 50%; the mass spectrometry conditions of the tandem mass spectrometry in the step (4) are as follows: Ion source type, namely electrospray ion source; Scanning mode, positive ion mode; Capillary voltage 3.0 kV; the desolventizing gas temperature is 500 ℃; the flow rate of the desolventizing agent is 600L/Hr; atomizer pressure 7.0 bar; Multiple Reaction Monitoring (MRM).
  2. 2. The method according to claim 1, wherein the shaking-up time in step (1) is 5min.
  3. 3. The method according to claim 1, wherein the high-speed shaking in the step (2) is carried out at a speed of 250 times/min for 2min, the rotational speed of centrifugation is 5000r/min, and the centrifugation time is 5min.
  4. 4. The method according to claim 1, wherein the vortex vibration in the step (3) is carried out at a speed of 250 times/min for 2min, the rotation speed of centrifugation is 5000r/min, the centrifugation time is 5min, and the filtration is carried out by using a microporous filter membrane, and the pore diameter is 0.22 μm.
  5. 5. The method according to claim 1, wherein the flow rate of the mobile phase in the high performance liquid chromatography in the step (4) is 0.3mL/min, the column temperature is 40 ℃, and the sample injection amount is 1.0. Mu.L.

Description

Determination method and application of enazachlor, florasulam and/or triazoxamide in feed Technical Field The invention relates to the technical field of pesticide residue detection, in particular to a method for measuring enazachlor, flumetsulam and/or triazoxamide in feed and application thereof. Background The clethodim is a novel acetaminophen herbicide and is mainly used for preventing and killing gramineous weeds and broadleaf weeds in corn and soybean fields. The cyprosulfamide is a second-generation sulfonamide herbicide for paddy fields, has extremely high control effect on annual weeds such as barnyard grass and the like and perennial difficult-to-control weeds, and has excellent effect on resistant weeds. The triazolyl oxamide is a triazolinone herbicide for paddy fields, has high efficiency on grassy weeds, annual weeds and annual broadleaf weeds, particularly has high efficiency on barnyard grass, has long lasting period, and is highly safe to apply even when rice is transplanted. At present, the three novel farmland herbicides are widely used abroad, especially in the grain crop planting process of rice, wheat, corn, soybean, sorghum and the like. These cereal crops are the main raw materials for making the feed, which results in a high probability of the presence of a large amount of residues of these three herbicides in the feed. The herbicide residues enter and are enriched in animal bodies through feeds, so that animal health is compromised, and meanwhile, the herbicide residues are ingested by human beings along with animal-derived foods, so that human health is compromised. At present, the European Union, the United states, japanese and other countries have regulated the residual limit of the three herbicides in plant-derived foods, for example, japanese regulated rice contains less than or equal to 0.05ppm of the florasulam and less than or equal to 0.05ppm of the triazoxamide, and European Union regulated fresh or frozen fruits, tuberous root and tuber vegetables, bulb vegetables, sunflower seeds, rapeseeds, soybeans, pumpkin seeds and corn grains contain less than or equal to 0.01ppm of the enazamide and tea leaves contain less than or equal to 0.05ppm of enazamide. Therefore, the residues of the three herbicides are harmful to human bodies, so that the method has important significance for the health of the cultured livestock and the safety of the food of human animal origin by measuring and controlling the residual amounts of the three herbicides in the feed. At present, the detection standard of herbicides in feed is less, wherein the purification technology based on gel chromatography is applied in the DB 34/T3102-2018 standard of measurement of sulfonylurea herbicides in feed-liquid chromatography tandem mass spectrometry, the operation is complex, the cost is high, a gel permeation chromatograph is needed to be purchased, the operation level of operators is required to be high, the detection range of the herbicide does not comprise three herbicides of clethodim, flusulfamethoxazole and triazoxamide, and the detection range of the herbicide is not suitable for three herbicides with high boiling point (425.7 ℃ to 550.8 ℃) detected by the invention in the GB/T23744-2009 standard of gas chromatography-mass spectrometry for measuring 36 pesticide residues in feed based on gas chromatography-mass spectrometry. At present, no corresponding detection method is available for the three novel herbicides, and the detection of the residues of the three herbicides in the feed is blank. Therefore, how to provide a method for rapidly and accurately determining the residual quantity of the florasulam, the enazachlor and the triazoxamide in the animal feed is a technical problem which needs to be solved by the technicians in the field. Disclosure of Invention In view of the above, the invention provides a method for determining enazachlor, flumetsulam and/or triazoxamide in feed and application thereof, which is based on a dispersion solid phase extraction pretreatment technology and combines ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) to rapidly and accurately determine whether the animal feed contains herbicide such as flumetsulam, enazachlor and triazoxamide and the corresponding residual quantity. In order to achieve the above purpose, the present invention adopts the following technical scheme: the method for determining the enazachlor, the florasulam and/or the triazoxamide in the feed comprises the following steps of: (1) Sample pretreatment, namely taking a sample to be detected, adding water, uniformly mixing, standing for 15-30min, adding an extraction solvent and a homogenizer, and shaking uniformly to obtain a primary extract; (2) Adsorption of impurities and water, namely adding an adsorbent into the primary extract, vibrating at high speed, centrifuging, and taking supernatant to obtain a secondary extract; (3) Purifying the extracting solutio