This standard specifies the determination method of six carbamate pesticide residues in grains and vegetables. This standard is applicable to the analysis of residues of cypermethrin, isoprocarb, propoxur, carbofuran, pirimicarb and carbaryl in grains and vegetables. GB/T 5009.104-2003 Determination of carbamate pesticide residues in plant foods GB/T5009.104-2003 Standard download decompression password: www.bzxz.net

ICS 67. 040
National Standard of the People's Republic of China
GB/T 5009.104—2003
Replaces GB14877-1994
Determinnation of carbamate pesticide residues in vegetable fouds
Issued on August 11, 2003
Ministry of Health of the People's Republic of China
Administrative Committee of Standardization of the People's Republic of China
Implemented on January 1, 2004
GB/T 500B,104——2003
This standard replaces GB114877—1994 Determination of carbamate pesticide residues in food. Compared with GB143771994, the main changes of this standard are as follows: the Chinese name of the standard has been modified, and the Chinese name of the standard has been changed to "Determination of residual amount of aminocarboxylic acid esters of pesticides in plant foods" 3. The structure of the original standard has been modified according to the standard CB/T2UU01.4·20014 Part 4: Chemical analysis method.
This standard was proposed and regulated by the Ministry of Health of the People's Republic of China. The drafting units of this standard are the Food Hygiene Supervision and Inspection Institute of the Ministry of Health and the Tianjin Food Hygiene Supervision and Inspection Institute. The main drafters of this standard are Fei Guangwei, Zhang Fuxia, Shui Rong and Li Mingyuan. The original standard was first issued in 1994, and this is the first subscription. 16
1 Model figure
GB/T5009.104——2003
Methods of aminocarboxylic acid esters of pesticides in plant foods Determination of Residue This standard specifies the determination of the residue of six kinds of nitrogen-based acid electrocides in grains and vegetables. This standard is applicable to the analysis of residues of sulfamethoxazole, isoflurane, carbofuran, anti-foam and carbofuran in grains and vegetables. The detection limits of this standard are .0.020, .02, .03, .15, .0.02, and .10 g/kg2 respectively. Principle
After separation, the organic compound is thermally decomposed on the surface of the heated alkaline plate to form a radical (N), and the atomic state of the metal (R) released by the heated metal surface is converted into (N) and combined with hydrogen. The ions are released to form positive ions in the alkaline chamber, which are collected and used as signal electrodes for determination. The current signal is positively correlated with the content of the nitrogen compound, and the quantitative comparison is carried out by negotiation. 3 Reagents
3. 1. Sodium sulfate hydrate, calcine at 450℃ for 1 h and set aside. 3.2. Redistill.
3. 3. Anhydrous methanol, redistilled.
3.4 ​​Dichloromethane: redistilled.
3.5 Petroleum ether boiling range 30~60℃ redistilled, 3.6 Sumitrocarb (sumi) purity 9%.
3.7 Isopropylamine (MIT): purity 299%:
3.8 Propoxur (propoxur>purity 99%
3.9 Arbofuran. Purity 99%, 3.10 Ri-iniuarb. Linearity s9% 3.11 Arhary1) purity 2-59%. 3.1250g/L sodium hydroxide solution, you lead to g sodium oxide, use water to dilute to 500mT..3.13 Methanol-salt Sodium chloride solution, take anhydrous methyl sulfoxide and 0/1.5% molten salt solution, 3.14 Preparation of carbamate insecticide standard: accurately prepare various standard products of fire-sensitive, isopropyl, residual, photosensitive, anti-inflammatory and methyl sulfoxide into 1mg/ml standard stock. When using, dilute the two methyl sulfoxides into single standard products (5g/mL) and mixed standard products (each concentration is 2%/ml.~10uR/mI.). 4 Apparatus
d.1 Gas chromatograph: with FTD (fire-screen thermal ion detector). 4.2 Electric bacteriostat,
4.3 Tissue precipitator,
4.4 Grain powder precipitator: with 20 days of precipitate. bZxz.net
4.5 Constant temperature water precipitator.
4.6 Pressurized concentrated gastric.
4.7 Liquid leakage 4250ml.inmmT.
4.8 Volume: 55m.15mL
GB/T5009.104—2003
4.9 Stopper flask: 250ml..
4.10 Flask: 250.
4.11 Full bucket, 10c.
5 Preparation of samples
Grains were crushed by food grinder and sieved for 2 days to make root food samples. Vegetables were removed from non-edible parts and the rest was crushed into tissues by crusher to make vegetable or tissue samples.
6 Analysis steps
6.1 Extraction
6.1.1 Food samples: Weigh about 40g of food samples, accurate to (1.90) and place in a 251ml micro-flask. Add 21~10% anhydrous sodium sulfate (depending on the moisture content of the sample) and 100% anhydrous methanol. Mix tightly, put in an electric vibrator and vibrate for 24 hours. Then filter through a rapid filter paper in a cylinder. Collect 51% of the filtrate and transfer it to a ml separating funnel. Wash the filtrate with 50ml TiO/T sodium oxide solution and put it into a separating funnel.
6.1.2 Vegetable samples: Weigh 20 Take the sample of vegetable and make it accurate to C, put 250 ml of GnR- in a stoppered bottle, add 80 ml of dead water with alcohol, tighten, and vibrate on an electric vibrator for 3min. Then, extract 200 ml of the sample through a quick filter, and wash the extraction bottle and the filter with 50 ml of anhydrous alcohol. Transfer the extracted liquid into a separatory funnel, wash the filter with 10ml 1.5% CHCl aqueous solution several times and put it into a separatory funnel. 6.2 Purification 6.2.1 Root food sample: add 50ml of isocyanate to a 250ml separatory funnel containing the sample extraction filter, incubate for 1 min, let stand for stratification, put the lower layer (methanol-sodium chloride solution) into the first 250ml separatory funnel, add 25mL methanol-sodium hydroxide solution to dry the methanol layer, shake until dense, let stand for stratification, and put the lower layer into the methanol-sodium hydroxide solution. 6.2.2 For the trial, add 50 mL sodium carbonate to the 500 mL separatory bucket containing the extract. Let it stand for 1 minute. After the layers are separated, place the lower layer in the first 500 mL separatory bucket and add 50 mL sodium carbonate. After the layers are separated for 1 minute, place the lower layer in the third 500 mL separatory bucket. Then add 25 mL of ethanol-sodium hydroxide solution and add it to the second separatory bucket. 6.3 Extract the sample into a separatory funnel filled with sample purification solution, extract with dihydromethane (53.25.25mL) once, shake for 1 min 4 times, and after static separation, transfer the dichloromethane to a 250 ml flask covered with anhydrous sodium sulfate (glass cotton) (pre-washed with dichloromethane), and rinse the funnel with a little dichloromethane and transfer it to the distillation flask. Connect the distillation flask to a melt pressure concentrator, concentrate to about 1 ml with water, add the distillation flask, transfer the residue to a 10-calibrated centrifuge tube, wash the hot plate repeatedly with dihydromethane and transfer it to the centrifuge tube. After the dichloromethane solvent is completely removed, dissolve the residual solution with acetone and determine the concentration to 2,400 ml for gas phase analysis. 6.4 Gas phase analysis conditions 6.4.1 Chromatographic column Note: Glass column, 3.2mm inner diameter × 2.1m, filled with 2% 0-16 + 1.5% 0-210 filtered fixed phase ChromasarhPis medium
Chromatographic column * Glass column, 3.2mm inner diameter × 1.5m, filled with Caromosorb WAUMS medium coated with 1.% 0-17 + 1.5% 0-210 mixed fixed phase.
6.4.2 Gas properties
Air 65ml./min, air 150ml./min, hydrogen 3.2mL/min6. 4. 3 Temperature properties
Column temperature 190℃; injection port temperature 310℃. 6.5 Determination of
Place one sample from each of the samples in step 6.3 into a gas chromatograph for chromatographic analysis: qualitatively compare the peak times on the two chromatograph rods with those of the standard part.Comparison between external standard method and standard correction method: The result calculation is as follows: In the formula, the content of the component in the standard sample is in grams per dry gram (n/kg). The unit of the content of the component in the standard test rod is nanogram (nm): The area or peak height of the component in the standard test rod is the unit of integration! Sample weight, unit is gram (R),
Injection volume (2.0m:1.)
Conversion unit
GH/T5009.104—2003
The absolute difference between two independent test results obtained under repeatability conditions shall not exceed 15% of the arithmetic half value. 9 Chromatogram of carbamate insecticide
Color multiple diagram must be 1
Taste extinguisher or,
Guide to the pesticide or!
-text or.
anti-good,
one foreign ban,
Note: No. 2FO1O-21CC0m00 (P8 mesh 100 mesh 21101 or 240X5.Raoge×Ci gas 65mL/min, air noon 1.50ml./min.hydrogen,a.2:ol/wu.surrounding 1 Six kinds of amino acid age resistant insecticide gas phase erotic surrounding 19
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