GB/T 5009.163-2003 Determination of multi-component residues of carbamate pesticides in animal foods by high performance liquid chromatography

This standard specifies the determination of aldicarb, metolcarb, carbofuran, carbaryl and isoprocarb residues in animal foods by high performance liquid chromatography. This standard is applicable to the determination of aldicarb, metolcarb, carbofuran, carbaryl and isoprocarb residues in meat, eggs and dairy products. The detection limits of this method are 9.8μg/kg for aldicarb, 7.8μg/kg for metolcarb, 7.3μg/kg for carbaryl, 3.2μg/kg for isoprocarb and 13.3μg/kg for isoprocarb. GB/T 5009.163-2003 Determination of multi-component residues of carbamate pesticides in animal foods by high performance liquid chromatography GB/T5009.163-2003 Standard download decompression password: www.bzxz.net

[CS 67.04]
National Standard of the People's Republic of China
GB/T 5009.163—2003
Determination of carbamate pesticides multiresidnernanimalfoodsHPLC)
2003-08-11 Issued
Ministry of Health and Family Planning of the People's Republic of China
China Trademark Promotion and Administration Commission
2004-01-01 Implementation
GH/T5009.163—2D03
This standard is for the determination method based on WHC/GFMS/FOOD: SeinwanilLnl, T1.: Pesticide ion General method for extraction and analysis of industrial chemicals, An1erm (198513:7524. This standard is not equivalent to the supplementary method recommended by WHO/GEMS/FOOE>. This standard is proposed and managed by the Ministry of Health of the People's Republic of China. The responsible units for the development of this standard are: Institute of Nutrition and Food Hygiene, Chinese Academy of Preventive Medicine, Beijing Municipal Health and Epidemic Prevention Station, and Food Hygiene Supervision and Inspection Institute of the Ministry of Health. The main drafters of this standard are: Li Ping, Wang Xuyu, Ling Guohua, and Gou Dajin. (8/503. 163—2003
Zhiweiwei, Didicarb, Shirandan. Ziweiwei and Isopropylamine are amino acid pesticides with a market share of 1.5% in my country. They are used for samples of animal food with special characteristics, and sample purification is one of the key technologies for the determination method. This standard proposes a method for the determination of the residual amount of Zhiweiwei, Didicarb, Shirandan and Isopropylamine in animal food by gel permeation purification technology: 1 Scope
Determination of amino acid pesticides in animal food by multidimensional separation and high performance liquid chromatography
8/T5009.163-2003
This standard specifies the screen liquid chromatography This method is applicable to the determination of isoprocarb in animal foods. The detection limits of this method are 9.0 g/kg for isoprocarb/13.2 g/kg for isoprocarb/13.2 g/kg for 1.2 g/kg for 1.3 g/kg for 1.5 g/kg for 2.5 g/kg for 2.5 g/kg for 3.5 g/kg for 1.2 ...1.2 g/kg for 2.5 g/kg for 3.5 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1.2 g/kg for 1. Methanol: redistilled.
3.2 Propylene glycol: redistilled,
3.3 Ethyl acetate: redistilled,
3.4 ​​Cyclohexane: redistilled,
3.5 Iron tantalum
3.6 Anhydrous sodium sulfate,
3.7 Distilled water: redistilled,
3.9 Standards for aminocarboxylic acid pesticides (NMC5): dimethoate, methylamine, methacrylic acid, quick-drying agent, isocarb The concentrations of the five NMCs were separated into: 1.0 mg/L, 5.0 m/L, 1.0 u/L, and 0.0 mg/L. 4.1 Commercial high-efficiency concentration phase chromatograph: attached with external detector and batch processor. 4.2 Transfer and evaporate.
4.3 Purification of coagulation chamber: 50cm long. 2.0cm inner diameter. 4.0cm thick. Use ethyl acetate to remove the colloid. The colloid has not been soaked in the liquid. 5 Sample preparation
After the egg product is shelled, it is quickly formed into a pulp. The meat product is ready for use. 6 Analysis steps
6. ! 6. 1.1 Weigh 20 mL of egg white (sugar content: 100 g), add 5 mL of water (depending on the water content of the sample). The total amount of water added is 2 mL. Egg white contains about 75% glycerol, add water and shake for 3 hours. Add sodium chloramine and stir until fully mixed. Add 3 mL of chloroform and shake for 30 minutes. 5m. above solution, rotate it in anhydrous steel, concentrate it, add 2ml ethyl acetate (1:1> melt chain, concentrate it again, repeat this process for 1 time, the concentration is about 1ml.6.12 Weigh 20g of meat sample, sieve it to the desired size. Add water (the standard water content of the sample is monohydrate, so that the total water content is about 2:1, the water content is about 7:1, the water content is about 1:1, the total water content is about 2:1, the total water content is about 7:1, the total water content is about 1:1, the total water content is about 2:1, the total water content is about 7:1, the total water content is about 1:1, the total water content is about 2:1, the total water content is about 7:1, the total water content is about 1:1, the total water content is about 1:1, the total water content is about 2:1, the total water content is about 1 ... 1 Extraction and distribution of egg samples.
6.2 Treatmentwww.bzxz.net
The pool was reduced and eluted with ethyl acetate-cyclohexane (1+=), 6 mL~35 mL fractions were discarded, 35 mL~75 mL fractions were collected, and the fractions were spun down to a concentration of about 1 mL. The fractions were then purified by a centrifuge and 35 mL~75 mL fractions were collected. The fractions were concentrated by rotary evaporation, and the volume was reduced to about 1 mL. The volume was made up to 1 mL with ethyl acetate, and the residue was subjected to HPLC analysis. 6.3 High-performance phase chromatography determination
E. 3.1 Chromatographic conditions
6.3.1.1 Chromatographic column Allylmcu4,umx r. 6.3.1.2 Dynamic phase, methanol-water (60+43), flow rate 0.5 mL/min. 6.3.1.3 Temperature increase
6.3.1.4 The external detection wavelength is 210 μL: 6.3.2 Determination
After adjusting the instrument to the state of mass, inject 5 ng of the source food standard and the test purification into the chromatographic device respectively to ensure the qualitative determination by comparing the peak height or peak area of ​​the sample with the standard. 6.3.3 Chromatographic diagram
The chromatogram is shown in Figure! :
Gradient formation:
2. ~ ~ extinguishing.
3—Made from carboxylic acid,
isopropyl,
Figure 1 Standard chromatogram of carboxylic acid ester pesticides
Result calculation
Format:
Wherein,
Xm.Vx100)
mx,x100u
.--The content of each pesticide in the sample, the unit is mg/kg; m---The content of each pesticide in the sample solution, the unit is mg/kg; m =Nanogram (Eg): m fiber mass, unit is gram)
V.-sample input position, single speed slightly open)
W: final volume of sample, unit is mI.) Calculation results retain two valid values,
8 Density
GA/T5009.163-2003
In the case of multiple pieces of material, the value of two independent determination results shall not exceed 15% of the technical average confidence:
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