This standard specifies the determination method of pesticide residues such as dichlorvos, acephate, demeton-methyl, phorate, monocrotophos, dimethoate, methyl parathion, malaxon, chlorpyrifos, methyl pirimiphos, fenthion, malathion, parathion, methidathion, chlorpyrifos, chloramidophos, ethion, malathion, parathion, methidathion, chloramidophos, ethion, chlorfenapyr, isoprocarb, fenbutylcarb, and carbaryl in grains and vegetables. This standard is applicable to the analysis of residues in grains, vegetables and other crops that have been treated with organophosphorus and carbamate pesticides such as dichlorvos. GB/T 5009.145-2003 Determination of multiple residues of organophosphorus and carbamate pesticides in plant-derived foods GB/T5009.145-2003 Standard download decompression password: www.bzxz.net

ICS 67.040
National Standard of the People's Republic of China
G8T5009.145—2003
GB/T17331—1558
Determiation of organophosphorus und carbamate pesticide muliresidues lt vegelable foods2003-08-11issued
Ministry of Health of the People's Republic of China
Standardization Administration of China
Implementation on January 1, 2004
GB/T5009.145—2003
This standard reorganizes GB/T17331299 Determination of multiple residues of organophosphorus and carbamate pesticides in foods. Compared with GB/T17831—1999, this standard has the following major changes: The Chinese name of the standard has been changed, and the Chinese name of the standard has been changed to "Determination of multiple residues of organophosphorus and carbamate pesticides in physical foods3",
GB8/T20002.42001≤Standard Compilation and Storage Rules Part 4: Chemical Analysis Methods The structure of the original standard has been modified
This new standard is issued and managed by the Ministry of Industry and Health of the People's Republic of China. The responsible institution for this standard is the Food Hygiene Supervision and Inspection Institute of the Ministry of Health. The main drafters of this standard are Zhang Zheng, Yang Huoxuan and Yi Rong. The original standard was issued in the autumn of 1993, and this standard is the first revision. 23
GB/T 5009.145—2003
Organic phosphine and aminomethanone pesticides are two types of pesticides with the fastest usage in my country. The method of multiple residue analysis of pesticides in real products can cover the residue analysis of multiple pesticides, and can solve the residue analysis of harmful components and unknown components of pesticides in food. This method provides multiple residue analysis of 16 organic enzymes such as dichlorvos and 4 aminomethanone pesticides such as cypermethrin in grains and vegetables, and is also suitable for the analysis of the residues of other organic phosphine and aminomethanone concentrates. 23
1 Scope
Organophosphorus and aminomethanone residues in plant foods The GE/T5009.145-2Q03 standard for determination of various residues of organophosphorus and amino methyl ester pesticides has been established. The standard has been set up to determine the residues of dimethoate, benzyl alcohol, methyl parathion, malathion, chlorpyrifos, methyl parathion, malathion, chlorpyrifos, fenthion, malathion, parathion, chlorpyrifos, chlorpyrifos, isoprocarb, sec-butyl, and chlorpyrifos in food and vegetables. This standard is applicable to the analysis of the residues of organophosphorus and amino methyl ester pesticides such as benzyl alcohol in grains, vegetables, etc. 2. The organic and amino methyl ester pesticides in the sample are extracted with an organic solvent, and then filtered, purified, and purified by a microcolumn to detect the residual substances, which are detected by a nitrogen-phosphorus detector (FTT). The qualitative analysis is based on the retention time of the chromatographic spectrum, and the quantitative analysis is based on the external standard method. 3 Reagents
3. 1 Indole: redistilled.
Methane monoxide re-ignited.
3.37. Dessiccant: redistilled.
Methanol, distilled.
N-hexane: redistilled.
Phosphoric acid,
Sodium chloride.
Anhydrous sodium sulfate.
Gel: 6-8 months 13n drying 2h, with 3% water to lose 3.11
Filter aid; celite545.
Gel, 5g ammonium chloride + 10ml. Phosphoric acid + 100ml water with 5 times pesticide standard, light 1.
Agricultural name
Demeton-methylamine
Shendingjian
Methyl meat fresh
Methyl mixed brand
Long-actingbZxz.net
English name
del:lirvux
Hrephrate
iroprccaub
demeton-methyt
phatate
munucrotphos
Ciaetboate
GB/T 5009. 145--2003
Agricultural contract name
Flowering (four-dimensional)
Methyl to use
and oxygen solution
Book death identification
Year-based teeth some whole
New like
For relatives
Cooking snail group
3.14 Agricultural to the preparation of standard solution
Table 1 (actual)
English name
urbaryl|| tt||paalnarznethy!
alztliur
ehtorpyrics
innupog
Feulion
malethicn
putptb:or.
wthid.tob
phetabiphos
tooth Accurately weigh the standard samples of table! Towel, use acetone as the solvent, prepare 1g/mL standard stock solution, store in the refrigerator, use the standard solution of each variety to dilute, and then according to the response ratio of each pesticide variety in the artificial soil, collect the standard solution of ten groups of plates, dilute and use the standard solution accurately. 4.1 Set the correct machine.
4.2 Xi heart machine,
ultrasonic cleaning group.
Rotating Fluid Insulator
Gas Detector with Nitrogen Phosphorus Detector (FID)
5 Preparation of Samples
Grind the food sample with a grinder, pass it through a 20-mesh sieve, remove the surface water, and sieve the edible part to make an analytical test.
6 Analysis Steps
6.1.1 Vegetables
6.1.1.1 Take 1 μg of sample in a conical flask, and the sum of the sample and water is equivalent to 10 ml of water and 20 ml of acetone. Vibrate for 10 minutes, pump out, take 2 ml, and transfer to the separator. 8.1.1.2 Weigh 5 g of sample (depending on the amount of pesticide in the test tube), put it in a 50101 centrifuge tube, add 10 ml of water with a water content of 1 g, and place it in a sterilizer. Ultrasonic extraction for 10 minutes: centrifuge at 5000 z/min to settle, and use a pipette to remove 10 ml of the liquid. 6.1.2 Weigh 20 g of sample in a centrifuge, add 5 g of sodium 100 sodium ionate. Take 30 ml of the sample and filter it in a centrifuge. Take 50 ml of the filtrate and transfer it to the separator.
6.2 Purification
Add 40mL of coagulant and 1g of attractant celite45 to the liquid separation tube of 6.1.1.1 or add 20mL of coagulant and 1g of attractant ueiie 545 to the liquid separation tube of 6.1.1.2. Place 5ml of coagulant on the bottom, pass through a Buchner filter with two layers of paper, and adjust a small amount of 3.96
CB/T 5009.145-2003
coagulant to wash the gel separation tube and cloth tube. Transfer the filtrate to a temperature hopper, add sodium chloride, extract with 5050.311, dichloromethane, combine the three extractions with chloroform, filter through a sodium sulfate funnel and put into a concentration bottle, concentrate to a small amount on a rotary evaporator at 36°C, dry with a bottle, remove the bottle, add a small amount of n-hexane, use a little cotton to seal the outlet of a 5m medical syringe, and wet the 1&silica gel with n-hexane, pour the liquid in the concentration bottle into the column, wash the concentration bottle with a small amount of hexane-dichloromethane (10 1), and pour it into the column. Wash with 4mL hexane + acetone (7-3) 4mL ethyl alcohol .8mL acetaldehyde acetyl ester (1-1) 4mL acetone + methanol (1-1) in sequence, and all the filtrate is concentrated by rotary evaporator at 45°C for nearly ten minutes, and the concentration is fixed to 1m[to 6.1.? The liquid should be added with 55mL.5 sodium hydroxide, then double 50mL.80mL. dimethylbenzene extraction twice, the dimethylbenzene layer is combined and dried over anhydrous steel, then shrunk on a rotary evaporator for 40 minutes in a water bath, and the concentration is 1ml. 6.3 Determination
6.3.1 Gas chromatography reference conditions
6.3.1.1 Chromatographic column, BP5 or OV-10125an×0.s%mm<inner diameter) quartz capillary. 6.3.1.2 Gas flow rate r
gas, 50mL/min;
tail gas (effective gas), 3mL/min
oxygen, 0.5kg/cm%
penetration point 0.3 ky/cm.
6.3,1.3 Short
Prevent leakage by using programmed humidity rise mode
voo/ari
Constant 2Dun2/in
6.3.1.4 Detection group: mouse phosphorus detector (F1D). 6.3.2 Chromatographic analysis
135℃
Icr/min
Function 1h
235℃Inlet temperature 240T
Measure 1% of the standard liquid sample and drip it into the chromatograph, and determine the quality by the retention time, and adjust by comparing the peak height or peak surface of the sample with the standard.
6. 3.3 Chromatogram
7 Result calculation
7. 1 Calculation
Calculate according to formula (1),
X =≤×Ex×1 000
hXm×t
X, one: 1 The content of organic pesticides in the component, in milligrams per dry gram (mg/ke? The height or peak area of ​​the main component in the test: one-the height or peak area of ​​the component in the standard: the content of the component in the standard sample, in nanograms (ng); : Test list, in grams (g);
F——conversion number, food is 173, vegetables is 2/3. 7.2 Precision and accurate medicine
16 kinds of organic pesticides and 16 kinds of oxyformic acid pesticides were added to the standard respectively, and the sugar density and accuracy test of the method were carried out in the addition recovery rate of 73.33%~105.22%. The required variation number was between 2.17% and 7.6% . 233
GB/T 5009. 1452003
2.0F2 methyl parathion
3.775 methyl parathion
4.097 trichlorfon 1
7.3 detection limit
detection limit see table 2,
6.163 1
-6.5 methyl endorphate
7.7W7 long-term efficacy,
lianglelai:
nongchenminghuai
modified mother
Z. methyl parathion
dihuowei
yedaogan
zhong qing
methyl endorphate
single Mengcheng
methyl endorphate
and blood||tt ||Methyl phosphorus
Fu Sui Xue
Ma controlled the neck fee
Happy speed Gu
Kill the pants
Gr. roasted library
Figure chromatogram
12.238 Ma protected true phosphorus,
12.745,
13.357 steam reduction
14.18 Methyl phthalate two:
14.853 with acid case!
14.847 Mala alkali screen
15.0? For or screen!
18.23 solution:
18.412 B bowl screen
21.293 g line screen,
minimum pick small who degree/ek>
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