GB/T 5009.20-2003 Determination of organophosphorus pesticide residues in food
Some standard content:
ECS67.040
National Standard of the People's Republic of China
GB/T5009.20—2003
Replaces G/T5C09.20—199%
Determination of organophosphorus pestiride residues in food Issued on August 11, 2003
Ministry of Health of the People's Republic of China
National Standardization Administration of China
Implementation on January 1, 2004
GB/T5009.20—2003
This standard replaces GB/T5009.20—200366 Determination of organic pesticide residues in food. The main changes compared with GB/T5909.20—196 are as follows: - The Chinese name of the standard has been modified, and the Chinese name of the standard has been changed to Determination of organic pesticide residues in food: The structure of the standard has been reorganized in accordance with GB/T2MM1.1—200361 Standard Preparation Rules Part 4: Chemical Analysis Methods 3.
This standard was proposed and managed by the Ministry of Health of the People's Republic of China. The first standard was drafted by the Analysis and Testing Center of the Chinese Academy of Agricultural Sciences, Beijing Agricultural University, and the Food Safety Inspection Institute of the Ministry of Health.
This standard was drafted by the Food Safety Inspection Institute of the Ministry of Health, Shanghai Municipal Health and Prevention Station, and Beijing Municipal Health and Epidemic Prevention Station. The first version of this standard was published by the Ministry of Health in 1952, revised for the first time in 1998, and revised for the second time in this year. 15
1 Specification
Determination of residual organic chain pesticides in food
GB/T5009.20—2003
Determination of residual organophosphorus pesticides in fruits, vegetables and cereals This standard specifies the residual organophosphorus pesticides in fruits, vegetables and cereals, such as electrophosphorus, quick-acting pesticides, long-acting pesticides, acetylcholine, chlorpyrifos, chlorpyrifos, methylsulfuron, chlorpyrifos, methylsulfuron, chlorpyrifos, chlorpyrifos, etc. The residual analysis method of phosphorus, ethoxyphosphorus, dimethoate, chlorpyrifos, thiophosphorus, and chlorpyrifos is used for the analysis of residual amounts of fruits, fruits, and crops that have been treated with twenty kinds of agricultural preparations such as chlorpyrifos, etc.: 2 Principle
Organic phosphorus-containing straw is burned in high-hydrogen-added fuel, and emits special light with a wavelength of 526 nm in the form of TIF fragments. After passing through a filter, the light is received by a photomultiplier, converted into a signal, and recorded by a micro-amplifier. The peak area or peak height of the sample is compared with the peak area or peak height of the standard for quantitative control: 3 Test
3.1 Propylene glycol
3.2 Dioxygen methyl alcohol
3.3 Sodium chloride
3.4 Anhydrous sulfuric acid
3.5 Filter aid Celite 515.
3.6 The standard pesticides are as follows:
DDVP: purity 99%
3.6.2 Rvinp: purity % trans-histamine
3.3 Ocophate: purity %
Pructuphus: purity %
Diszinn: purity 9%.
Ethyl sulfide erimfos: pure 9%
Pirishosethyl: purity ss% methyl-.hin-: purity.
Kitazine: purity 99%
Amine isrmh: purity:
Po-gnelog pure%
Pe1thoate, pure 9.6%.
Medium thion (1 purity 99.6%.
Eanips: pure 2.99.9%
Ethion (HM) purity 9
Dimethoate linethat purity 99.0
Purity 98.2%
Micro (Hin), pure%.
GB/T 5009.20--2003
3.6.20 Phosphate (enitmthion purity 3.5%). 3.7 Preparation of pesticide standard solution: Accurately weigh the standard substances of 3.6.1~3.6.20, use methyl chloride as solvent, prepare 1.0mg/mL standard solution, store in refrigerator at 4℃, and absorb the response of each pesticide to be collected by the instrument at any time, absorb the standard solution in a constant amount, and dilute it with methane to form a mixed standard solution. 4.1 Thermal crusher
4. 2 4.3 Heat treatment and extraction 4.4 Gas phase chromatograph (FPL) 5 Preparation of samples Take grain samples and grind them into powder, then sieve them to make grain samples, remove the non-edible parts and make analytical samples. 6 Analysis steps 6.1 Collection 6.1.1 Fruits and vegetables Weigh 50.0 μg of sample, put it into a 300 μm beaker, add 5 mL of water and 1 mL of propane (the total volume of the extraction is 15 cm3), and extract it in a microfuge for 1 min to 2 min. Filter it with a filter funnel with two layers of filter paper and 10 g of Celite 545, and transfer the extracted mL to a 50 mL microfuge: 6.2 Grains Weigh 25.0 μg of sample. The sample is weighed in 300 L of flask, and 100 1 ml of water and acetone are added. The following steps are the same as 5.1. 1.6.2 Purification
6.1.1 5.1.2 Add 0-15% sodium hydroxide to the liquid to make the sample saturated with acetone. Vibrate vigorously for 2min-3min, let stand for 3min, separate the acetone and the water phase, and use 50ml of the water phase. Vibrate with ethane for 2min: let stand for stratification again, extract the acetone with methane, filter it, and dehydrate it through a glass funnel filled with 20g-106 anhydrous ethanol. Filter it into a 25mL filter bottle, and then wash the container with about 40mL of dichloroethane with anhydrous sodium sulfate. The washing liquid is also added to the flask, concentrated to about 2% by condenser evaporator, and then transferred to a 5-25mL bottle of dichloroethane. Determine by gas chromatography
6.3 .1 Reference conditions for rapid spectrum
6.3.1.1 Chromatographic column
a) Glass column 2.6m×mm(id), filled with ChrurausorhWAWDMICS (A month ~ IC month) containing 4.% DC-200+2.5CV-17
b) Column 2.6m×3wm(id), filled with QF-1 with a mass fraction of 1.5% (hrmml:WAW6
6.3.1.2 Gas velocity
Hydrogen=0ml./min.Climate=1ccml./min.Nuclear gas=0cml./min.6, 3.1.3 Temperature
24℃, vaporization chamber 260, detection fee 27.6.4 Determination
Pipette 2μ~ standard wave and sample purification solution and inject them into the chromatograph to determine the retention time. Compare the sample's drop or selectivity with the standard solution, and calculate the result. The content of the organic matter of the component is calculated according to formula (1). =
A, × V, x V × F, X1 000
AX: ×V XX1 530
: The content of the organic phosphorus compound, in ng/kg; In the sample: The peak area of the component, in units of integration; In the mixed standard solution: The peak area of the component, in units of integration: The total volume of the actual sample solution, in units of traces (mL); The total volume of the extract for purification, in units of milliliters (mL); The fixed volume after the extraction, in units of millilitersThe color increase diagram, the ground is around 1. li
Respect the low inspection record, thank you 3.2xllwng/kg
This screen-off low exchange specific validity: mg/
Long-term research avoidance low test soft risk 2,>14mgkg select low test heat Xia./kg
Ba minimum degree of stimulation 0.11/kg
Secondly, the low detection chain (.(IC4mg/kg=B event bed sensor low protection test selection U.0c3u.g/bg hand complete low degree 00G
risk most period test heat quality 0.00%/g
Pursue the most false exchange filter concentration retreat 0, nn4TR/kR;求皮肤释放磷低整通实建0.ou>格kg
车化4确定降量低协池证惠0.U2Gkgm帮丰放避低检测利效片0.017mg/kzl座流降最低空利集中0.514mg/kg:克我最低检测性皮5.5mg/kzl
助低3.21mg/kg
Figure 116和Organic hard pesticides (standard case addiction) chromatogram of the country 161
GB/15009.20—2003
9.213 Organophosphorus pesticides chromatogram Figure
13 kinds of organic waste concentrated pesticides color chart, see Figure 2. L
Cause fear;
2-A selection,
3--Two must run;
One sleep light energy:
A beauty eyelash dye;
Irregular rice epidemic:
10 Fan lice
Le Le;
Only tax secret:
Thai convection screen:
Kill before the report!
B system,
Figure 213 kinds of organophosphorus pesticides chromatogram
Second method of organophosphorus pesticides in grain, vegetables and oil This standard specifies the determination of residual amount in grains, vegetables, edible oil, malarial phosphorus, chlorpyrifos, chlorpyrifos, chlorpyrifos, etc. The method is applicable to the residual amount analysis of grains, vegetables, edible oil, malarial phosphorus, chlorpyrifos, chlorpyrifos, chlorpyrifos, etc. The output limit is 0, 1, 3, the input sample is equivalent to 0 sample, the minimum detection limit is o, olm/ks--c.oma/kR.
11 principle
CB/T 5009.20—2003
The organic surfactant in the sample is extracted, separated and purified, and then burned on a hydrogen-rich filter. The FL1 () fragment emits a 526nm long light. This and the characteristic light are selected by the filter and received by the photomultiplier. It is converted into an electrical signal and amplified by a micro-current amplifier and recorded. The total sample height is compared with the standard peak height to calculate the equivalent rat 12 reagent in the sample
12. 12.2 Anhydrous sodium sulfate.
12.3 Propylene glycol.
12.4 Neutralization agent: for chromatography, 10u activation 1b and set aside. 12.5 Propylene charcoal: weigh 20% sodium charcoal and soak overnight, pump full, wash until there is no chloride ion. Bake at 12u for use,
12.6 Sodium sulfate (5) g/L)
12.7 Pesticide standard solution: accurately weigh an appropriate amount of organophosphorus pesticide standard solution, mix with rice (or methane) to the reserve supplier, and store in the refrigerator.
12.8 Pesticide suspension solution: Temporarily use dioxygen to release the solution to a concentration of 100%. Malathion, parathion and carbamate are equivalent to 0.0 ... Add 3-58 grams of methane: add 7 grams of methane: add 100 grams of methane to the container, add 0.00 grams of neutral calcium oxide, add 20 grams of methane, add 3.5 grams of methane, filter through a paper filter, take 35 mL of methane, evaporate naturally at room temperature in a ventilated environment until the residue is precipitated with a small amount of methyl chloride several times, transfer to a 1m15) scale test container, and make up to 2.1. Reserve: 14.1.2 Hull the rice, grind it, pass through a 20-piece sieve, and filter it. Collect 10.00 g of the October rate bottle, add 0.00 grams of neutral calcium oxide to 20 methane, add 3.5 grams of methane, multiply the amount by 301 m) of methane, and measure 5 mL of the liquid to make up to 2.1 mL. 14.1.3 Corn: Grind the test material into 21% powder, mix it: Take 1g.95 and put it in a stoppered bottle, add 0.5g of lead, 0.2L of hot water and 2L of oxygen, shake for 05h, filter the liquid and inject it directly. If the amount of the test material is too low, add 30L of dioxane. Remove the heat and filter, add 15ml of concentrated liquid and make up to 2mL. Injection: 14.1.4 Weigh 5.0% of the test material into the control pool, dissolve it with 50.0% acetylene and wash it with 10mL of water. Gently transfer it to the sample pool and separate it for 1m. Let it stand for more than 1 minute, discard the oil layer below, and let the upper layer separate by itself. Use a separatory funnel. Be careful not to use excess reagent. (If the separation is serious, add 50ml of clear liquid.) In the centrifugal agitator, add 0.5 mL of the upper layer containing 1% sodium bicarbonate (50 g/mL) and 1 mL of dichloromethane (25 g/mL). After stratification, take the concentrated portion and transfer it to a flask. Extract the tremella with 10 ml of 1% fluoromethane for 1 time. After separation, mix until the hair becomes clear naturally. If there is no water, use a small amount of "floating methane" to extract the residual amount and transfer it to a container. Add 2 ml of sodium sulfate to dehydrate, add 1 g of aluminum oxide and 0.2 g of activated carbon (3 g can be added to remove oil and color). After natural separation, filter and add directly into a single liquid. If there is little water in the dihydrogen fluoride, you can use 5 ml of chloroform to extract the residual liquid after evaporation into a small separator in batches. Take 1min, and after the separation, transfer the dichloromethane layer into a container, extract once with 5mL dichloromethane, add the mixture to a container with equal concentration, make the volume to 1ml, and shake to remove water with anhydrous sodium hygroscopic acid. Add 1g neutral alumina and 0.2g activated carbon, remove oil and color, filter and select. Or pour the dichloromethane and the mixture into a container, evaporate with dichloromethane, add the precipitate into a container, take the dichloromethane layer as the standard, and add 3% anhydrous sodium hygroscopic acid, then print neutral alumina and activated carbon on it. Operation 14.2 Chromatographic New Parts
14. 2.1 Column: glass, inner diameter 1 mm, reflection 1.5 m -2.0 T. 14.2.1.1 Separation and determination of chromatographic column: a) 2.5-3.0 mm thick (100-200 μm) chromatographic column with a fixed microstructure of 2.5% E30 and 1.5% QF-1; b) 2.5-3.0 mm thick (100-200 μm) chromatographic column with a fixed microstructure of 60-80 μm (200-300 μm) mixed with 1.5% V-17 and 1.5% QF-1. 14.2.1.2 Separation and determination of chromatographic column with stirring, electrophoresis, addition of iodine, dark reading and frequency conversion. ) The interior of the microscope is coated with a fixed solution of 3PEA and %QF-I. ) The interior of the microscope is coated with a fixed solution of 2%NPGA and 3%QF-1. 14.2.2 The gas flow rate is: carrier gas is oxygen 80m:./min, air 5mL/min, oxygen 180mL/min, the ratio of carrier gas to oxygen is not selective. 14.2.3 Temperature: Inlet: 220, detector, 240, temperature: 180℃, but the determination of dichlorvos is 130%. 15 Specifications: 2.3 The standard pesticides are injected into the gas phase negative spectrum collector at 2K.*. The peak heights of the standard organic phosphorus solutions with different concentrations can be measured to prepare the standard organic phosphorus lines respectively. At the same time, take a sample and inject it into the gas chromatograph. The measured drop is still from the standard line. 15 Calculation
The content of organic pesticide in the sample is calculated according to formula (2. A×1c3wwW.bzxz.Net
R×1000×1000
In the formula,
is the content of organic pesticide in the sample.The content of organic phosphorus pesticide in the sample volume is expressed in milligrams per gram (mg/k). The unit is nanometers; the sample volume (L) is equivalent to the mass of the sample. The unit is grams (R). The calculation results retain two effective digits. The absolute values of the two independent determination results of formaldehyde, dithiothreitol and trithiothreitol under heavy conditions cannot be calculated by arithmetic. 0%
Lexing, parathion and chlorpyrifos were obtained under repeatability conditions, and the absolute difference between the two independent green nests did not exceed the calculated average
16 other
gas chromatograms of other organic pesticides, Figure 3.~Figure 5164
2.536SE30 and 3-fold QF1, 180T: second bottle
parathion
Gas chromatogram of 33 kinds of organic pesticides in China G-1#
Methacrylic acid:
Degree of purity:
Multiple sparseness:
Gas chromatogram of 54 kinds of organophosphorus pesticides Figure 1
GB/T5009.20—2003
.-temperature
Figure 4 Gas chromatogram of multifunctional pesticides
2NPGA-SSQF||t t||Animal:
Thick invitation net,
3.--Dirty alcohol
Kill shrimps and crows,
Original 6, 4 kinds of regulated drugs with gas color entry: 1ss
GB/T5009.20-2003
19 Scope
Method 3 The determination standard of organophosphorus pesticide residues in meat and fish stipulates the residual analysis method of organophosphorus pesticide residues in meat, fish and fish. This standard is applicable to the residual analysis of organophosphorus pesticide residues in meat and fish. The detection limits of dichlorvos, dimethoate, malathion and parathion are 5.0.3, 0.015, 0.015 and c.335 mg/kg respectively. 20 Principle
Same as in No. 2:
21 Test solution
21.1 Propanol
21.2 Dichloromethane.
21.3 Anhydrous acid solution: calcine at 700°C for 1 h and set aside. 21.4 Neutral sodium oxide: calcine at 550°C for 4 h
21.5 Sodium hydroxide solution (20°C).
21.6 Standard pesticide liquid: Accurately weigh 10.0m3 of parathion, dimethoate, carbon monoxide, and parathion, dilute with acetone to 100m3, mix evenly. 0.10mR of each milliliter of pesticide is used as a catalyst. Keep 21.2 Standard pesticides on ice for one month. Dilute with two drops of water to a density equivalent to 100ml before use. .0, 22 Apparatus
22.1 Chromatography: with flame photometer (FI3). 22.2 Electric analyzer
23 Analytical steps
23.1 Purification
Put the chemically active substance into a 2501ml conical flask, add 50mL of acetonitrile and shake thoroughly (1.5h, filter it). Take 12ml of the separated liquid. Add 50mL of magnesium sulfate solution (20g/L) and 10mL of fluoroform. After shaking for 2min, monitor the stratification. Collect the lower layer and add 12ml of the extract into a bucket. Then use 20% dihydrogen peroxide to extract the acetonitrile solution in the same way. Extract it twice. Take out the bottle and add 1 ml of oxygen (if it is added, add 1.5 g), shake several times, and add 20% anhydrous sodium sulfate. Vibrate to dehydrate, pass through the algae, wash with 2 ml of methane in two portions, put it into the evaporator, and evaporate it to 1 m. In the evaporator, add the residual solution several times to the scale test tube, adjust it to 2 mL 5 mL. If the probe contains a little water, add a small amount of sodium hydroxide in the evaporator, wash it again with honey and put it into the scale test tube, and adjust it to 2 mL 5 mL. 23.2 Chromatographic conditions
23.2.1 Chromatographic column: glass column with an inner diameter of 3.2 mm and a length of 1.6 m, filled with 5oH-100% Chromosorb with a constant flow rate of 1.5% (V-17) and 2% QF1 wAwLiMcs.23.2.2 Flow rate nitrogen, 5)ml/min: hydrogen, kg/cm: air. 5kg/eu23.2.3 Temperature, test needs 25), injection port 250%℃, column benefit 22℃ (measurement time is 140%): if the company has completed the measurement of the four pesticides in the market, use the program temperature rise,
23.2.4 The color bands of 4 kinds of organophosphorus pesticides are broken, and the chromatograms of 4 organophosphorus pesticides are determined by 7.165
1-ene,
R-lakpi:
23.3 Specifically determine the chromatograms of 4 organophosphorus pesticides
GM/5009.20—2003
Use the standard or sample injection: mT.~3L, use the retention time to qualitatively measure the peak height, and compare it with the standard dimension for early determination. 24 Calculation of results
Same as the first?
25 Density
The absolute difference between the results of the two independent determinations obtained under the vertical compression test shall not exceed 1% of the average value of the method.On the right, add the residual product to the scale test tube several times, and adjust it to 2mL5mL. If the probe contains a little water, add a small amount of sodium hydroxide in the evaporation medium, and then wash it with honey in the scale test tube. 23.2 Chromatographic conditions
23.2.1 Chromatographic column: Glass column with an inner diameter of 3.2mm and a length of 1.6m, filled with 5oH-100% Chromosorb with a constant flow of 1.5% (V-17) and 2% QF1 wAwLiMcs.23.2.2 Flow rate nitrogen, 5)ml/min: hydrogen, kg/cm: air. 5kg/eu23.2.3 Temperature, test needs 25), injection port 250%℃, column benefit 22℃ (measurement time is 140%): if the company has completed the measurement of the four pesticides in the market, use the program temperature rise,
23.2.4 The color bands of 4 kinds of organophosphorus pesticides are broken, and the chromatograms of 4 organophosphorus pesticides are determined by 7.165
1-ene,
R-lakpi:
23.3 Specifically determine the chromatograms of 4 organophosphorus pesticides
GM/5009.20—2003
Use the standard or sample injection: mT.~3L, use the retention time to qualitatively measure the peak height, and compare it with the standard dimension for early determination. 24 Calculation of results
Same as the first?
25 Density
The absolute difference between the results of the two independent determinations obtained under the vertical compression test shall not exceed 1% of the average value of the method.On the right, add the residual product to the scale test tube several times, and adjust it to 2mL5mL. If the probe contains a little water, add a small amount of sodium hydroxide in the evaporation medium, and then wash it with honey in the scale test tube. 23.2 Chromatographic conditions
23.2.1 Chromatographic column: Glass column with an inner diameter of 3.2mm and a length of 1.6m, filled with 5oH-100% Chromosorb with a constant flow of 1.5% (V-17) and 2% QF1 wAwLiMcs.23.2.2 Flow rate nitrogen, 5)ml/min: hydrogen, kg/cm: air. 5kg/eu23.2.3 Temperature, test needs 25), injection port 250%℃, column benefit 22℃ (measurement time is 140%): if the company has completed the measurement of the four pesticides in the market, use the program temperature rise,
23.2.4 The color bands of 4 kinds of organophosphorus pesticides are broken, and the chromatograms of 4 organophosphorus pesticides are determined by 7.165
1-ene,
R-lakpi:
23.3 Specifically determine the chromatograms of 4 organophosphorus pesticides
GM/5009.20—2003
Use the standard or sample injection: mT.~3L, use the retention time to qualitatively measure the peak height, and compare it with the standard dimension for early determination. 24 Calculation of results
Same as the first?
25 Density
The absolute difference between the results of the two independent determinations obtained under the vertical compression test shall not exceed 1% of the average value of the method.
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.