This standard specifies the determination method for the residues of pesticides such as α-666, β-666, γ-666, δ-666, heptachlor, aldrin, p,p-DDT, p,p-DDD, p,p-DDE, o,p-DDT, cypermethrin, cyhalothrin, permethrin, cypermethrin, cypermethrin, cypermethrin, deltamethrin, etc. in grains and vegetables. This standard is applicable to the analysis of the residues of grains, vegetables and other crops that have been treated with organochlorine and pyrethroid pesticides such as 666. GB/T 5009.146-2003 Determination of multiple residues of organochlorine and pyrethroid pesticides in plant foods GB/T5009.146-2003 Standard download decompression password: www.bzxz.net

ICS 67.640
National Standard of the People's Republic of China
GB/T5009.146--2003
Replaces GB/T17332-1998
Deterrninatlon of organochlarines and pyrethroidperticide maltiresidues in vegetable foods2003-08-11Promulgated
Ministry of Health of the People's Republic of China
National Standardization Administration of China
Implemented on 2004-01-01
B/T 5009. 146---2003
This standard recommends CB/T17332-199R Determination of multiple residues of organochlarines and pyrethroidperticide maltiresidues in food2. Compared with B/117332-1998, the main changes of this standard are as follows: 1. The Chinese name of the standard is changed to the determination of various residues of organic and technical pesticides in plant foods:
. 2. The original standard is modified in accordance with CB/T30007.4-2001 Standard Preparation Plan Part 4: Chemical Analysis Methods.
This standard is issued by the Ministry of Health of the People's Republic of China. The relevant units are the Health Inspection Institute of the Ministry of Health, the Ministry of Health, the Ministry of Agriculture and Rural Affairs, the Ministry of Health, and the Ministry of Agriculture.
This standard is issued by the Ministry of Health of the People's Republic of China. The original standard was published in 1995. This standard is for the preparation of a second edition. GB/T 5009.146-2a03-34 Organochlorine and pyrethroid pesticides are the two most common pesticides in China. The method for analyzing the residues of pesticides in food covers the analysis of the residues of various pesticides. It can solve the analysis of zero components and unknown components of pesticides in food. This standard provides a reference for the analysis of the residues of 11 chlorinated pesticides such as 6666 and 6 pyrethroid pesticides such as chlorpyrifos. It is also suitable for the analysis of the residues of chlorinated pesticides and pyrethroid pesticides. GB/T 242-142 Determination of the residues of organochlorine and pyrethroid pesticides in food of physical nature. 5009,146—2003
This standard specifies the determination method of pesticide residues in grains and vegetables, including 665.566.8665.76 ... 3.1 Petroleum ether boiling range 50℃~~90℃ redistillation: 3.2 Benzene.
3.3: Distillation,
3.4 ​​Ethyl acetate, redistillation.
3.5 Anhydrous thiourea,
3.6 Flory bond, layer break, butyl 520% ​​average 4 after standby, 11C drying for 2 hours before use, add 5% water to inactivate 3.7 Pesticide standard, see Table 1.
Pesticide name
Pp\-Didi
Wine wine
, ndi
A sail chrysanthemum
Daidonglin
Cyanothrin
Australian and New Zealand pepper
English name
. p-TYT
Pp-DDT
e,p'DDT
beptachlor
skrir:
fenpropathurin
eyaalarhrn
prrmrthrin
rygermetht:n
fea:valwr:itr
Jelaineirir
GB/T 5009.146—2003
3.8 Preparation of standard whole microparticles
Accurately weigh the standards in Table 1 respectively, dissolve them in benzene and prepare a 1 mg/mL stock solution. When using, dilute them with petroleum aldehyde to make a single-variety standard working solution. Then, according to the sound conditions of each pesticide on the instrument, different standard reserves are taken, and the petroleum aldehyde is mixed with the standard liquid.
A.1 Gas chromatograph: with electron capture detector (ECD). 4.2 Electric magnetic separator
4.3 Woven crusher.
and rotary hair analyzer,
the instrument: Buchner funnel (diameter 0mm) suction bottle (200ml), one corner of which is 15
4.7 Bono funnel: 250ml
4.8 Chromatographic column,
|5 Test preparationbzxZ.net
Take the grain containing the sample and crush it into grain sample by grain crusher, and then make it into grain sample. After 20 months, the sample is cleaned and the non-toxic part is removed for use.
6 Analysis steps
6.1 Extraction
6.1.1 Grain sample, weigh 10g of food sample, put it into a 103mL sealed flask, add 20ml of 1% acetone, and stir for 0.5h.
6.1.2 Vegetable sample, weigh 2ug of vegetable sample. Put it into a tissue crusher, add 30ml of acetone and 33ml of petroleum ether, crush it on a crusher for 2min. Then extract the mixture, filter it into a 250ml separatory funnel, add 10ml of 20k/T sodium sulfonate aqueous solution, stir it thoroughly, and separate the layers. Transfer the lower layer into a 250mL separatory funnel, collect it with 20ml of 20ml of 1% ethanol, combine the extracted petroleum ether layers, filter through anhydrous sulfuric acid layers, and concentrate to 10mL on an evaporator. 6.2 Purification
6.2.1 Preparation of chromatography column: Fill the column with 1 cm high anhydrous argon, then add 5% aqueous desinfluene and finally add 1 cm high anhydrous sulfuric acid. Gently squeeze, elute the purification column with 20 mL of industrial petroleum ether, remove the eluent, and leave a small amount of solvent.
6.2.2 Purification and concentration: Accurately pipette 2 mL of sample extract and add it to the purified column that has been eluted. Elute with 10% petroleum aldehyde + ethyl acetate (95 + 5). Collect the eluted solution in a steaming bottle, dry the liquid on a rotary precipitator until almost 10% oil is decomposed with a small amount of petroleum aldehyde in a graduated centrifuge tube and determine the maximum concentration to 1.0 ml for gas chromatography analysis. 6.3 Determination
6.3.1 Gas chromatography parameters Conditions
6.3.1.1 Chromatographic analysis: elastic capillary tube, 0.25mm (inner diameter) × 15m, with OV-101 stationary phase. 6.3.1.2 Gas flow rate, nitrogen: 40mL/min + tail gas. 6JmL/min ratio 1.55. 6.3.1.3 Measurement: temperature rises from 180℃ to 23U℃ and maintains for 301min, detection %, inlet temperature 2C℃ 6.3.2 Spectral analysis, absorption 11. The sample liquid is loaded into the gas chromatograph, and the retention time and peak height of the color peak are recorded. Then absorb: 1. The standard liquid is injected, and the detailed time and peak height of the color peak are recorded. According to the ratio of the peak time of the chromatograph on the chromatograph to the standard component, the quantitative analysis is carried out by external standard method and the standard component,
B. 3. 3 Spectrum
See the figure! 、
# 665;
--r665:
Supporting agent:
7 DE:
gP-DD
Three yellow sea (large)
13-bone enzyme:
Han ticket two wine.
7 purple fruit calculation
The following formula is used to calculate:
pressure 1 organic oxygen known insect poison standard color enhancement bacteria XEx
The content of pesticides in the sample, the unit is dry (/) nuclear push product: the content of pesticides in the component, the unit is the final volume (: the injection volume of the test is in microliters ();
final volume, the unit is milliliter (mL); loose standard product: the peak quotient of the component pesticide, the unit is meter (mm): the peak height of the pesticide in a sample, the median is the water (m) the residual of the group, the unit is
GDT50C9,146——2003
CB/T 5009.146-2003
Special times,
Precision and accuracy
Ten kinds of organic hydrogen and six kinds of chrysanthemum pesticides were mixed and spiked into flour and lycopersicum oil for viscosity and accuracy test. The recovery rate of addition was between 81.7% and 112.41%, and the coefficient of variation was between 2.48% and 19.05%.9
Detection limit
Detection limit was 2.
Agricultural name
Aldrin
PA-DUE
ap-DTYT
P,P: DDD
Pp'DNT
Purple mushroom
Ol'Pu
Detection limit g/kg
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