This standard specifies the determination method for multi-component residues of 13 commonly used organophosphorus pesticides in animal foods, including methamidophos, dichlorvos, acephate, monocrotophos, dimethoate, ethion, methyl parathion, fenitrothion, methyl pirimiphos, malathion, fenthion, parathion, and ethion. This standard is applicable to the determination method for multi-component residues of 13 commonly used organophosphorus pesticides in livestock and poultry meat and its products, milk and dairy products, eggs and egg products. GB/T 5009.161-2003 Determination of multi-component residues of organophosphorus pesticides in animal foods GB/T5009.161-2003 Standard download decompression password: www.bzxz.net

ICS 67. 040
National Standard of the People's Republic of China
GB/T5009.161—2003
Determinition of organophosphorus pesticidemultiresidues in animal foods
Determininalion of organophosphorus pesticidemultiresidues in animal foods2003-08-11Promulgated
Ministry of Health of the People's Republic of China
Standardization Administration of the People's Republic of China
Implementation on 2004-01-01
GB/T5009,161—2003
This standard corresponds to the determination method recommended by DIN EN/GEMS/FOOD: Sieinwundter, H., Methods for analysis of pesticide residues and industrial chemicals. Anal Chem (1985) 322: 752-751. This standard is not equivalent to the consistency of the determination method derived from WHO/C:EMS/FCOT. This standard is also issued by the Ministry of Health of the People's Republic of China. The originators of this standard are: Institute of Nutrition and Food Industry, Chinese Academy of Preventive Medicine. Ministry of Health Inspection Institute, Beijing Municipal Bureau of Food and Drug Control,
The main authors of this standard are Chen Huanjing, Yang Dajin, and Wu Guohua. GB/T 5009.16120G3
Organic pesticides are a type of pesticide commonly used in agriculture in China. Due to the lack of quality of animal food, the test method is one of the related technologies for the determination of animal food. This standard presents the data on the determination of 13 kinds of organic compounds in the restricted use products including acetylmuramic acid, dimethoate, chlorpyrifos, mannitol, thiabendazim, chlorpyrifos, dichlorvos, etc. in mice. 1 Scope
Determination of multi-component residues of extreme phosphorus pesticides in animal foods
GD/F5009.161—2003
This standard introduces the determination method for 13 commonly used organic group pesticides such as methylamine, dimethoate, chlorpyrifos, mefenamic acid, methyl pyrimidine, methyl pyrimidine, dimethoate, chlorpyrifos, and iodine in animal foods. This standard is also applicable to the determination method for 11 commonly used organic group pesticides such as methylamine, dimethoate, chlorpyrifos, methyl pyrimidine, methyl pyrimidine, methyl pyrimidine, marathion, chlorpyrifos, and acetyl iodine in fresh meat and its products, milk and dairy products, eggs and egg products.
The detection limits (g/g) of this method are: 5 g/l for methyl amine, 3.5 g for 10 g for 12 g for 15 g for 20 g for 25 g for 30 g for 40 g for 50 g for 60 g for 70 g for 80 g for 90 g for 100 g for 200 g for 250 g for 300 g for 400 g for 80 g for 60 g for 70 g for 80 g for 90 g for 100 g for 200 g for 200 g for 200 g for 300 g for 400 g for 80 g for 60 g for 70 g for 80 g for 90 g for 100 g for 200 g for 200 g for 300 g for 400 g for 80 g for 80 g for 70 g for 80 g for 90 g for 100 g for 200 g for 200 g for 300 g for 300 g for 400 g for 80 g for 80 g for 80 g for 100 g for 200 g for 200 g for 300 g for 300 g for 400 g for 80 g for 80 g for 80 g for 100 g for 200 g for 3 ...
3.2 Second order dishes..
3.3 Ethyl acetate: steamed.
3.4 ​​Cyclobene: steamed beans.
3.5 Hydrogenated chain.
3.6 Monosodium benzoate.
3.7 Condensation, Bi0BetsSX220~4003.8 Standard stock of organic phosphorus pesticides: see Table 1. 3.9 Standard stock solution of organic phosphorus pesticides: see Table 1. 3.9 Standard stock solution of organic phosphorus pesticides: accurately weigh 25ml of each organic phosphorus pesticide sample (0.0010ml) and dissolve in 25ml of ester of acid in a bottle and make up to volume (each is /m). 3.9.2 Standard stock solution of mixed organic phosphorus pesticides: before 20 minutes, measure each monomer organic phosphorus pesticide sample as shown below: Prepare the drug (3.9.1) in a 10 mL volumetric volume, blow off the solvent with nitrogen, and use the fresh milk that has been sensitized and purified in 5.2.3 and 5.3 to extract the diluted pesticide. The standard concentration of each organophosphorus pesticide in this filtration flow (4 g/m[.]) is: methyl parathion 16. modified chlorpyrifos 0. acetyl methoxychlor 24. dimethoate B, malathion 15. ethyl thiocarb 21. monobasic phosphorus 16. sodium thiocarb 15. chlorpyrifos 24. dimethoate 16. ethyl thiocarb 8.
GB/T5009.161-2003
Concentration name
Formic acid cream
Acetophos
Main obstacle
B parallel
A very strong against her casting
Kill secret release
Adenosine
Ma Luhao
Multiple frequency
Research
B Wei Confirm
4 Quick Agency
Table 1 Pesticide Standards
Secretion Text Good
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dichlneyss
aprjplhale
J:w:wLtu haplos
mountain
dieultateou
J:vethypgreth.an
Eenitrc.thion
piriruphais methyl
g.blathion
fenthion
parathson
erhinn
4.1 Gas chromatograph: with flame photometric detector, capillary chromatograph, 4.2 Rotary chromatograph.
4.3 Gel purification: K30en1, inner diameter 2.5m, with a glass plug, a little glass wool at the bottom, and a wet gel was loaded with ethyl acetate (1 + 1 1) elution solution. The gel bed was kept in the eluent for about 25cm. 5. Analysis step
5. Sample preparation
Salt products were shelled and made into slurry; meat products were cut into small pieces and made into meat paste; dairy products were mixed with melon 5. 2 Extraction and separation
5.2.1 Weigh 20g of egg sample (decocted to 0.01g) and put it into a 100mL flask. Add 5mL of water (add water according to the water content of the sample, the total amount is about 20g), add 40mL of acetonitrile, add 6mL of sodium hygrometer for 10min, shake thoroughly, then add 30mL of dichloromethane, shake for 3min, take 3ml of the above solution, put it into a rotary evaporator with anhydrous sodium sulfate, concentrate to about 1mL, add 2mL of acetic acid, cyclohexane (1+1) to dilute it, repeat this process 3 times, and finally concentrate to about 1ml. 5.2.2 Weigh 20g of egg sample (accurate to 0.11g), add 6mL of water (add water according to the water content, the total amount is about 20g), and mix according to 5.2.1 Egg samples were all taken and the distribution steps were performed. 5.2.3 Weigh 20g of milk sample (accurate to 0.11*), and follow the steps of 2.1 for egg sample collection and distribution: 5.3 Purification: Cut the sample into pieces and elute with 7.7% cyclopentane (1:1) solution, discard 0mL~35mL of the fraction, and flask 35mL~7uml of the fraction, and spin the elution to about 1mL, and then purify it with a multi-column to collect 35mL~7uml of the fraction, and obtain the elution. Collect the fraction until 1mL, and adjust the volume to 1ml with acetic acid, and leave it for GC analysis. 5.4 Gas chromatography determination 5.4.1 Hazard spectrum equipment 5.4.1.1 Chromatographic sample: coated with S54 (0.25μm, Hm×0.2mm inner diameter) stone elastic fine column, 5.4.1.2 Wet: steady ascending speed for 60min 5.4.1.3 Inlet temperature: 270℃. 235℃/265℃ 5.4.1.4 Detector: flame detector (EP-P), GB/T5009.161—2003 5.4.1.5 Gas flow rate: carrier gas: 1mL/min; induction: 50mL/min; hydrogen: 50ml./min, air: 500anL/min. 5.4.2 Chromatographic analysis: Take 1 μl of the mixed standard solution and the sample purification flow respectively and inject them into the chromatograph. The qualitative analysis is based on the retention time and the order is determined by comparing the peak drop or peak area between the sample and the standard. 5.4.3 Chromatogram
See Figure 1.
1---Methyl link:
Ethyl link;
Ethyl link;
Methyl link,
9-killing bullet
insect end Xue,
pregnant pull blue screen:
Ge Bing Kang
Figure F13 kinds of organic selenium pesticide chromatogram
6 Chu fruit calculation
Calculate according to the formula:
In the formula:
X=thermal XV×1
mX ×1 000
The amount of each pesticide in the sample, in milligrams per kilogram (mg/kg); the content of each pesticide in the test solution, in nanograms (g); 30
GB/T5009.161—2003
-Test item, in grams (g);
V-calibration injection volume, in liters (
V, the final volume of the sample is in liters (mL). The calculation result is rounded to two significant figures.
Precision clinical
The difference between the results of two independent determinations obtained under reproducible conditions shall not exceed 15% of the arithmetic mean.
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