ECS 67.040
National Standard of the People's Republic of China
GB/T5009.126-2003
Replacement GH/T14973-199-
Determination of triadimefon residues in vegetable foods2003-08-11Promulgated
Ministry of Health of the People's Republic of China
National Standardization Administration of China
2004-01-01Implementation
bzxz.netGB/T 5009.126--20G9
This standard replaces GB/T14973
19944 Determination of residual amount of hydroxyl radical in food 3. Compared with GB/T14973-1994, this standard mainly changes the standard name as follows: the Chinese name of the standard is Determination of dihydrogen sulfide residues in physical food; according to the writing rules of GB/20001.4--2013 standard, Section 4: Chemical analysis method, the structure of the original standard is reversed. Therefore, this standard is proposed by the Ministry of Industry and Information Technology of the People's Republic of China and is under the jurisdiction of Jiangsu Agricultural University. The main drafters of this standard are Liu Yibian and Ying Jian. The original standard was first issued in 199, and this is the first revision. 12.1 Scope Determination of triadimefon in plant foods This standard specifies the determination method of triadimefon residues in food and fruit. This standard is applicable to the determination of triadimefon residues in root foods, vegetables and fruits that have been treated with triadimefon. The detection limit of this method is 2.8×10,2 Principle Triadimefon residues in the sample are determined by gas chromatography after purification. CB/T5009.126—2003 The detection end has good sensitivity to triadimefon: triadimefon and its main metabolite hydroxycarboxin react with ascorbic acid vapor to produce CN- ion flow, which causes the electrical signal received by the detector to change. This change process is recorded, and the peak heights of triadimefon and hydroxycarboxin on the sample chromatogram are compared with the chromatogram of the standard sample to calculate the triadimefon residue. Mountain bee, crazy sequence, trimethoate, hydroxycarboxin,
3 Reagents
3.1 Propylene glycol.
3.2 Chloromethane.
3.3 Sodium oxide.
3.4 Anhydrous sodium sulfate, 500 degrees Celsius for 4 hours.
3.5 Wedding frying.
3.6 Chloroform.
3.7 Florisil + (orisil) 60 days--100 days, 650% drying for 5 hours, add 3.5% water to dehydrate, transfer to 4 days--6 days3.8
Standard pesticide reduction
Precisely weigh 50.0 mg of triazole (iriailirlnm) and 1riadiruuaul standard crystals. Add acetone to dissolve, and make up to 100.0 mL respectively. As the preparation solution, store in the refrigerator. This solution is equivalent to triazole per milliliter to form 1riadiruuaul ECF. When using, take equal amounts of triazole and sodium chloride stock solution, mix them, and dilute them step by step with internal resistance as the use medium. The concentration of triazole and 1riadiruuaul is generally 1. og/n11.
4 Instruments
4.1 Small grain crusher
4.2 High-speed tissue crusher.
4.3 Ultraviolet or hygroscopic vibrator
4.4 Rotary evaporator.
4.5 Gas chromatograph, nitrogen detector and microcomputer 5 Analysis steps
5.1 Extraction
5.1.1 Grain: weigh 30.0g of flour after 10 days, put it in a 500ml Erlenmeyer flask, add 80mL of acetone and 20mL of water, let it stand overnight, extract it with an oscillator for 1h, filter it, wash it with 30w:L and 30mL of propylene, combine the extract and washing liquid, and dry it on a rotary evaporator (water content 0- 45, the same below), after removing most of the propane, move to a 2m[separating bucket, add 2
GH/15003.126-2003
5Cml. hot water, 10ml. sodium chloride aqueous solution, 0ml monochloroethane in sequence, stir for 2m, let stand and separate, transfer the lower organic phase to a conical flask, extract the water phase with 20ml. methyl chloride once. Discard the water phase, and dehydrate the combined organic phase with anhydrous sodium sulfate. <Anhydrous sodium 10R left stone> After collecting 250m polymer, condense and shrink, and then form a new shape. Use a small amount of acetone to hydrolyze the dichloroethane. Wash the pear-shaped bottle several times, and collect the makeup in the test tube. Use the quality control agent to determine the quality of the product! , and measure the color of the color.
5.1,2 Fruits and vegetables: weigh the sample crushed by the chain weaving machine and add 57.0B into a 300m bottle, add 1 active ingredient %, 800ml of acetone, extract on a generator for 10min, add 0.01ml of acetone overnight, extract with a generator for 30min. Wash the residual liquid and container with 20mL.25mL of acetone, combine the extract and washing liquid, and gradually concentrate to 1(i0ml) on the generator. Add silica to the split funnel, add 30ml of distilled water, 12ml of sodium hydroxide and 40ml of dimethylformamide, and press 5,1. 1\ shake for 2 minutes and then change the mixture. 5.2 Clean the mixture. If the determination result is affected by the bees, it can be further purified by chromatography. The inner diameter of the column is 1.2 cm, and the flat part is 20 cm long. Add 1 cm high anhydrous sodium sulfate and 1% activated carbon (mass fraction). 1. Add 1% anhydrous sodium sulfate and 1% ... 5.3 Gas phase chromatographic analysis
5.3.1 Chromatographic toxicity
5.3.1.1 Chromatographic column: inner bell 5m, length 1.6m, corrugated glass: filled with 80H-JocHCrotmnaorl, WAW-TMCS, with 4% 0V-17 and 4% 0V-2[0 combined with kitchen extension
5.3.1.2 Gas flow plate: carrier gas is oxygen 70m/mn, hydrogen 3.6mL/min, air 16mml/min5.3.1.3 Temperature source 220, vaporizing air (inlet 323: detection chamber 2905.3.2 Determination and calculation
Separately inject the pesticide standard sample and the test sample into the gas phase instrument, and the external standard curve method is used. Calculate the triketone residue according to the following formula Retention amount: X=(-6)XVX1003
or:
A--Retention amount of a sample, in mg/mL (tnR/kR), L--Diazole concentration in sample solution, in μg/mL (E/mL), C
V--Test volume after sample solution, in μL (L)--Test rod mass, in grams (g). The calculation results are numerical, and the precision is 10% of the average value of the two consecutive samplings under the condition of gravity. The chromatogram of
7.1 (concentration 1μg/mL, minus 16) is shown in Figure 1.
4.625Diazolopyridine
5,092According to the specification and specification, the sample is generally not subjected to column purification. However, if column purification is required, different batches of florisil should be pre-eluted to ensure that the bag medicine is recovered.
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