GB/T 5009.162-2003 Determination of multi-component residues of organochlorine pesticides and pyrethroid pesticides in animal foods

This standard is applicable to 20 commonly used organochlorine pesticides and pyrethroids such as α-HCH, β-HCH, γ-HCH, δ-HCH, pentachloronitrobenzene, heptachlor, heptachlor epoxide, aldrin, chloranil, cypermethrin, p,p-DDE, p,p-DDD, o,p-DDT, p,p-DDT, tetramethrin, permethrin, cypermethrin, α-cypermethrin, deltamethrin, etc. in meat, eggs and dairy animal foods. GB/T 5009.162-2003 Determination of multi-component residues of organochlorine pesticides and pyrethroid pesticides in animal foods GB/T5009.162-2003 Standard download decompression password: www.bzxz.net

JCS67,04g
National Standard of the People's Republic of China
GB/T5009,162--2003
Determination of organuchlurine and pyrethroid pesticides mulairesidues in animal foods2003-08-11Promulgated
Ministry of Health of the People's Republic of China
National Standards Committee of the People's Republic of China
2004-01-01Implementation
GB/T5009.162-2003
This standard specifies the following methods for the extraction and analysis of pesticides or industrial chemicals recommended by WHO/GEMS/FORD: Standard Method for Extraction and Analysis of Pesticides or Industrial Chemicals: 4ru lChr1l (19851522:732-754, the degree of consistency of this standard with the determination method recommended by WHO/GEMS/FCKUL is non-effective. This standard was proposed by the Ministry of Health of the People's Republic of China and is under the jurisdiction of the relevant units, including the Chinese Institute of Preventive Medicine and Food Hygiene, Beijing Municipal Health and Prevention Station, and the Ministry of Health's Health Supervision and Inspection Institute.
The main drafters of this standard are Chen Lijing, Tu Taqing, Liu Hongzhi, Wu Guohua, and Yang Dajin. GB/T 5009.162—2003
Organic oxygen pesticides and pyrethroid pesticides are two types of pesticides used in my country. Due to the particularity of animal food matrix, the determination of sample chemical residues is one of the key technologies. This standard proposes a method for the determination of multi-component residues of n-HCH, PHCH, HCH, 8-TICTI, pentachlorobenzene, nitrogen, thiophene oxide, aldrin, chlorpyrifos, paracetamol, paracetamol, pyrethroids, PTFE ... 162—2003
This standard specifies the determination methods for two commonly used organic pesticides and insecticide-requiring alcohol pesticides such as α-TICII, 3-TICII, Y-HCH.8·HC.H, five-type reproductive energy, heptachlor, heptachlor epoxide, aldrin, calcium-induced chloramphenicol, end-dip dapoxetine, P·P-LDDE, PDL>).0P-DT, 2:-TDT, clothing, chlorine porridge, chlorine gas chrysanthemum prevention, oxygen deficiency chrysanthemum elimination, and beard meal belt pair in animal products. This standard is suitable for the analysis of various pesticides and pyrethroid pesticide residues such as α-IICH, 3HCH, 7-HCH, HCH, pentachlorobenzene, L-chlorobenzene, heptachlor epoxide, stearyl alcohol, chloranil, chlorpyrifos, doxorubicin, KP\-DE,\-FT, Jn\E>T. ammonium ester, chloranil, 4-cyanopyran, cyanamide, etc. in porcine energy foods. The formula of this formula is as follows: e-hexachlorocyclohexane 0.25 hexachlorocyclohexane 0.50; Y-hexachlorocyclohexane 0.1 hexachlorocyclohexane 0.25 pentane 0.25; cyclohexane 9.50 cyclohexane 0.0 cyclohexane 0.25; cyclohexane 0.50 cyclohexane 1.2 cyclohexane 3.25 [-DDTC 0.0 -TD 0.50 -DDE 0.50 1PD DD DU 75 12.57 2.C: 5-pi 2.50 deoxynivalenol 2.50,
2 principle
The sample is extracted, purified, concentrated, and fixed to volume, separated by a paper column gas chromatograph, and detected by an electron-assisted detector, and the retention time is used for qualitative analysis. External standard method. Decomposition: HCH, BHCH, -ICH, pentachlorobenzene, 1FH, heptachlor, aniline, end-treatment, cyclohexane, fusin, PP-DDE, P-TDTH), -bamboo T, Pp'-DDT, brain cat, complex energy, chlorinated chlorpyrifos, liquid chrysanthemum.
3 Reagents
3. 1 Propylene: heat.
3.2 Distilled methane. Trichoderma,
3.3 Ethyl acetate: egg vegetable.
3.4 ​​Hexane, calcined, heated to 400 °C,
3.5 n-hexane: precipitate:
3.6 Petroleum ether: analytical grade, 30 °C ~ 60 °C, direct distillation, 3.7 Sodium chloride,
3.8 Anhydrous sodium sulfate
3.9 Glue Hin·eaals$X, 200 liters-month: 3.10 Pesticide standard catalytic agent 1.
3.11 Preparation of standard promotion solution
Accurately weigh the substances in Table 1, dissolve them with a little benzene, and then use n-hexane to make the stock solution with the correct concentration. According to the equipment conditions, the standard chamber is prepared according to the manufacturer's specifications. 951 GB/T 5009. 162-2003. Name of agricultural product: 666-3666- ... List of pesticide standards
Pp'-DDE
quir.luzene
beplachbor
hepracdot epozide
skerin
dieldrin
Icngonwww.bzxz.net
nhlyrfrnsnn
Fnthalthrin
rmathrin
eypermethrm
fealvnlerate
dd:arine Jrin
4.1 Gas chromatograph: electron beam detector: capillary chromatograph. 4.2 Rotary evaporator
4.3 Gel purification: 302m diameter 2.5cml instrument required for shear chromatography, add a little glass wool at the bottom. The eluent was ethyl acetate and cyclohexane (1 + 1). The gelatin content was about 26cTl. The gelatin content was always kept in the special desorbent. 5 Analysis steps 5.1 Sample preparation 5.2 Extraction and distribution 5.2.1 Weigh 20g of egg sample (accurate to 0.0g) in 100mL. Add 5ml of water to the sample. Add water to make the total water content about 2C. Add 5ml of water to make the water content of the sample about 75%. 4g of acetone solution 30ml, add 6g of chlorinated acetonitrile, fully spread: add 3U mL of silica gel, shake for 30min. Take 35mL of the supernatant and filter it. After diluting with anhydrous sulfuric acid, transfer it to a condensation bottle and reduce it to about 1ml. mT. ethyl aldehyde cyclopentane (1 + 1 liquid) and then shrink, repeat this 3 times until it shrinks to about 1ml. 5.2.2 Weigh 20g of meat sample (accurate to 0.01g). Add 6mL of water (add water according to the moisture content of the sample to make the total water content about 20g. Generally, the moisture content of fresh meat should be 70%, so add 5ml of water). The following is the extraction and distribution steps of 52.1 egg sample. 5.2.3 Weigh 20g of milk sample (accurate to 0.01g. Fresh milk does not need to be added with water, and acetone is directly added for extraction. 1 The following is the non-extraction and dead-end treatment of egg sample in 5.2.1. 5009.162—2003
Then the fraction was selectively eluted with ethyl acetate-cyclohexane (1-1> ethyl acetate) solution, and 0.1ml~35ml fractions were removed, and 35ml-70ml fractions were collected. The fractions were then transferred to a 1ml column and purified by gelatinization to collect 35mL-70mL fractions. The fractions were evaporated and condensed to 1ml using hydrogen gas as the solvent and petroleum aldehyde as the solvent, and then the fractions were analyzed. 5.4 Determination
5.4.1 Gas chromatography conditions
5.4.1.1 Chromatography: 1V-10.25 mt:m0.2mm internal source) quartz crystal without emission,
5.4,1.2 Reduction: ascending order
wt/mn.283ttemin
170m35
5,4,1,3 Sampling full scale; 270℃
5.4.1.4 Detection of the core pin detector (E core 1). 300℃5.4.1.5 Carrier gas flow: Nitrogen (N): 1mL/min Blow t5umL/nim5.4.2 Chromatographic analysis
Respectively collect 1 mixed standard and test consumption purification belt controlled gas phase chromatograph, set the beat with the maintenance time, and compare the total peak area of ​​the new standard peak with the test result.
5.4.3 Chromatographic analysis
See Figure 1 for the chromatogram
6 Result calculation
Compare the following formula,
XmVX1050
m×X1oap
2-The content of each pesticide in the sample, the unit is grams per kilogram (m2/kg)m--The content of each pesticide in the sample liquid, the unit is nanometer (ng); the sample mass, the unit is grams
with the liquid sample material, single effect large combustion A) t——sample volume at the maximum point, the unit is litre (nl). The result must be calculated to ensure two valid digits. The precision must not be lower than the arithmetic mean of the results obtained under the gravity point. B/T5009.162—2003. 0.666 upper and lower six ...
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