This standard specifies the determination method of cypermethrin, fenvalerate and deltamethrin in cereals and vegetables. This standard is applicable to the multi-residue analysis of cypermethrin, fenvalerate and deltamethrin in cereals and vegetables. The detection limits of this standard for grains and vegetables are 2.1μg/kg for cypermethrin, 3.1μg/kg for fenvalerate and 0.88μg/kg for deltamethrin. GB/T 5009.110-2003 Determination of residues of cypermethrin, fenvalerate and deltamethrin in plant foods GB/T5009.110-2003 Standard download decompression password: www.bzxz.net

3CS67.040
Heart 53
National Standard of the People's Republic of China
GB/T5009.1102003
Recommended GB/T 14929.41994
Determination of cypermethrin,fenvalerate anddeltemethrin residues In vegetable foods2003-08-11Promulgated
Ministry of Health of the People's Republic of China
National Standardization Administration
2004-01-01Implementation
GB/T 5009.110—2003
This standard replaces GB/T14929.4—1994. Determination of the content of 4-hydroxy-2-thiazolinone, 2-hydroxy-2-thiazolinone and 2-hydroxy-2-thiazolinone in foods. Compared with GB/T14929.4—1994, the main revisions of this standard are as follows: The Chinese name of the standard is changed to "Determination of the content of 4-hydroxy-2-thiazolinone, 2-hydroxy-2-thiazolinone and 2-hydroxy-2-thiazolinone in foods of plant origin". The structure of the original standard is modified according to the fourth section of the rules for standard preparation of GB/T20001.4--2001: Chemical analysis methods. This standard is proposed and coordinated by the Ministry of Health of the People's Republic of China. The drafting units of this standard are: Guangdong Provincial Food Hygiene Supervision and Inspection Institute, Beijing Municipal Health Prevention and Control Station, and Food Hygiene Supervision and Inspection Institute of the Ministry of Health. The main drafters of this standard are Gong Dichen and Zhang Bixia. The original standard was first issued in 1994, and this is the first revision. 46
1 Scope
GB/T 5009.110--2003
Determination of flumethrin, cypermethrin and chlorpyrifos residues in plant foods
This standard specifies the determination method of flumethrin, chlorpyrifos and chlorpyrifos residues in vegetable foods and vegetables. This standard is applicable to the analysis of flumethrin residues in cereals, rice and vegetable food. The detection limit of chlorpyrifos in this standard is 2. 1g/kg. Pentylene ester. is 3, 1\g/kg. Dissolved cyanide chrysanthemum crystal is 0.88Jg/kg 2 Normative reference documents
The clauses in the following documents become the clauses of this standard through reference. For any out-of-date reference documents, all subsequent amendments or revisions are not applicable to this standard. However, the parties to the agreement on this standard shall study whether the latest version of this document can be used as soon as possible. For any out-of-date reference documents, their latest versions are applicable to this standard. GB: T5009.19: Determination of 666 and 1,200 mg/kg of hexachlorobenzene in sweet potato GH500, 200 mg/kg of determination of residual pesticides in food 3 Principle
Chlorhexyl acrylate, chlorpyrifos and chrysanthemum oxychloride are mixed, purified and condensed, and then determined by electron capture gas chromatography. After separation by a Bronze column, chloranthene, chrysanthemum and chrysanthemum fragments are put into an electron capture gun detector to measure their contents. The signal is put into a recorder to record the peak distance or peak area, and the peak height/peak product of the measured object is compared with the peak height or peak area of ​​the standard to determine the content.
4 Reagents
4.1 White oil aldehyde: 30%-60℃ quantitative distillation
4.2 Internal preparation:
4.3 Anhydrous chrysanthemum sulfate: 55l 4.4 Chromatographic medium: n 4.4 Chromatographic medium: n 4.5 calcined: h for use, baked at 11℃ for 1h before use. 3% water for deactivation. 4.5 Layer of carbon: 553 (burned for 1 hour and set aside. 4.6 Defining cotton: washed with n-alkane and set aside. 4.7 Standard drug:
Cypermethrin purity 96: Eua purity s%
Eliamethrir purity 07.5%. 4.8 Preparation of standard solution: Prepare 13/m2 of chrysanthemum ester 410-gmL and 10-gmL of cyanide solution respectively with distilled or prepared 15ml. Chlorine oxide sieve. 15 mi. The standard of chloranthracene, 5mL of chloranthracene was taken in a 25mL volumetric flask, and the standard was used as the standard. The concentration of chloranthracene was 16×10 g/mL, and the ratio of chloranthracene was 2×10 g/mL.
5 Receiver
5.1 Gas scanning spectroscopy detector. 47
GB/F5009.110--2003
5.2 High-speed tissue culture machine.
5.3 Electric embedding machine,
5. 4 High temperature furnace,
5.5K [concentrator or constant source water bath.
5.6 Binghan two-angle grid bottle,
5.7 Glass grip bucket.
5.810 injection.
Right analysis step
6. 1 Extraction
6.1.1 Rice: Weigh 10g of the crushed sample and put it into a 10mL tight conical flask, add 25mL of petroleum aldehyde. Vibrate for 33min or fill it with water. Take 2mL-4mL of the supernatant and pass it through a column (equivalent to 1-2g of sample). 6.1.2 If necessary, weigh 20g of the sample after slurry treatment and put it into a 230mL stoppered conical flask, add 4mL of acetone and petroleum aldehyde respectively. After 3min, let them separate, take out the supernatant and pass it through a column. 6.2 Purification
6.2.1 Rice: Use a glass chromatography column with an inner diameter of 1.5cm and a length of 25cm-30cm. The bottom is plugged with the necessary elution agent. Add 4mL of the supernatant from bottom to top as needed. 1cm of sodium sulfate, 3cm of neutral iodine, 2cm of anhydrous sodium sulfate, and then eluted the column with 10L of sodium sulfate. Discard the washing liquid, and when the aldehydes have dropped to the anhydrous sodium sulfate layer, quickly add the sample to the anhydrous sodium sulfate layer, add the washing current at a constant rate, and use 25m~8m of oxygen to elute. Collect the filtered water in a fixed bottle. After expansion, use nitrogen flow to 111L for gas chromatography. wwW.bzxz.Net
6.2.2 Flour and corn: The purification method used is the same as that in 6.2.1, except that 0.01L of chromatographic activated carbon powder is added to the neutral iodine layer (the amount of chromatographic activated carbon powder can be appropriately increased or decreased depending on the color depth) for decolorization operation in the same way as 6, 2.1. 6. 2.3 For dyes, the purification method used is the same as that in 5.2.1: add 0.022~1.03 chromatographic active powder on the neutral calcium layer (the amount of chromatographic active powder can be appropriately increased or decreased depending on the color depth) for chromatography, the amount of eluent used is 3nml.~33ml. No oil awakening, cooling operation is the same as 5.3.1,
6.3 Determination
Gas chromatograph with ELD,
5.3.1 Chromatographic equipment
6.3.1.1 Chromatographic column: glass 31tuu inner diameter>×1.m or 2m, filled with 3% () V-101/(chromoorbW (AWMCS) 8/19.
6.3.1.2 Temperature: 245% for the air pan, 260℃ for the sample inlet and detector 6.3.1.3 Gas: high-efficiency gas washing speed 110m/mn Result calculation
Use the external standard method to calculate:
Wu,
The content of the drug in the sample is in milligrams per gram (n/kg); c
The peak height of the test solution is in millimeters (mm); h,
The density of the standard liquid is in grams per liter (mg/mL); The injection volume of the standard solution is in grams per liter (mg/mL); =Liter [.]; The fixed volume of the sample, the unit is liter (mL.) 48
, - Standard drop peak height, the unit is mm [nn] Sample mass. The unit is g ()
- Test depth filter inlet plate, the unit is micron () 8 Sugar density
GB/T5009.110-2003
The absolute difference between the results of two independent determinations obtained under repeated comparison conditions shall not exceed 10% of the arithmetic value 9 The chromatograms of chlorpyrifos, chlorpyrifos and chlorpyrifos are shown in Figure 1.
1 - Aid
Monochlorpyrifos, confidentiality interval 2 min 57 sF3 Mouse matching · preservation time min50s
Convenience preservation 4
Figure 1 Chromatographic analysis
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