GB/T 5009.21-2003 Determination of carbaryl residues in grains, oils and vegetables
Some standard content:
IC5 67.040
National Standard of the People's Republic of China
GB/T5009.21—2003
Replaces GBT500S.2.1996
Determination of carharyl residues in cereals, oils and vegelable2003-08-11Published
Ministry of Education of the People's Republic of China
China National Standards Administration
2004-01-01Implementation
GEI/T 5009.21—2003
This standard replaces R/T5005.21935 Grain and Oil, Method for Determination of Carbaryl Residues in Food and Oil 3. Compared with GB/T5009.21·1996, the main changes in this standard are as follows: the Chinese name of the standard is modified, and the Chinese name of the standard is changed to GB/T2:111.1—20014 Standard Writing Rules: Chemical Analysis Methods The original standard structure is revised.
This standard is proposed and drafted by the Ministry of Health of China. The first standard is drafted by the Zhejiang Provincial Institute of Science and Technology, the Ministry of Health, and the Institute of Nutrition and Food Research, Chinese Academy of Medical Sciences.
The second standard was first marketed in 1985, 1! ! 6 years, the first revision, this is the first revision, 17m
Determination of rust residue in grain, oil, grain, this standard specifies the determination method of amine residue in grain, oil, vegetable, this standard specifies the determination method of amine residue in grain, oil, vegetable, vegetable, this standard specifies the determination method of amine residue in grain, oil, vegetable, vegetable, vegetable, this standard specifies the determination method of amine residue in grain, oil, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable, vegetable
3.2 Ethyl acetate.
3.3 Formaldehyde.
3.4-.Mature methane,
3.5 Sodium phosphate: 125%+drying 4
5.6% sodium phosphate: 123% mass fraction, after overnight storage, use 3.7H or 3.7H to prepare the standard product: accurately weigh the formaldehyde content (uruary.99,3): the alcohol in the solution is prepared into 1C, mg/L standard preparation, storage under ice. Use the standard that the formaldehyde release is [og/L] 4.1 High performance liquid chromatography: 4.2 Pass the reagent through an energy device with an external detector, 4.3 Ultrasonic collector, 4.4 KD compressor or rotary incinerator 5 Analysis step 5.1 Extraction The grain sample that has been sieved by 2U.J1 powder is placed in a 2E1) Til bottle, accurately extract with 150-17% water, soak overnight, extract for 1h, and select the appropriate amount. 5.2 Purification Take a 3cm diameter column, put it in a light-absorbing bucket, and fill the column with 2cm sodium hyaluronate at both ends and 6cm silica in the middle. The column was first prepared with 1m chromatographic column, and the dihydrogen methyl group was gradually removed. The sample was extracted and poured into the chromatographic column. The whole methyl group was washed with KD shrinkage for a period of time until nearly ten (water bath temperature 30°C), and then the solution or residue was collected and fixed at 5°C. After the final determination by C.45 micropore method, 1% of the juice was taken and the effective color band was measured. CB/T5009.21—2003 5.3 Phase chromatographic determination parameters 5.3.1 Chromatographic column: stainless steel column p-rrpak (u3.9mm×30 cm. 5.3.2 Detector, external detection end 280 ntm. Sensitivity n.01~-c, 32.5.3.3 Flow: Z. Disinfectant water (E5145) mixed flux, washing rate 1L/n. 5.3.4 Temperature,
5. 4 Determination
Accept 101. Standard use to change the sample quality, to ensure the quality of the time, monthly standard fear legal plate, 6 results
The content of methyl methacrylate in grain is calculated by formula (1): AXIoUu
×V/V,×1 000
Wherein;
X—…the content of formaldehyde in food, in milligrams per gram (mg/kg); the mass of sample to be calculated using the standard curve, in micrograms (μg); the volume of sample solution to be fixed to volume, in milliliters (mL); the volume of injected chromatogram, in mL; W.
7Other
quantities to be estimated, in units of steps
The chromatogram of formaldehyde is shown in Figure 1.
National 1 methyl methacrylate color standard diagram
...-(I)
Day principle
Method 2 colorimetric method
GB/T5009.21—2003
Under sensitive conditions, methyl methacrylate is hydrolyzed into 1-hydroxy-1-hydroxy-2 ...
9. 6 Petroleum aldehyde, boiling point 30℃--50℃.
Tris(II) iodide
Ca(II) oxide,
9.9 Silica gel.
Diethylene glycol diacetate, diethylene glycol dichloride and dichloromethane (10%)
Coagulation solution: Take C5R carrier and dissolve it in 4 ml of water, add 1 ml of phosphoric acid (10%). Potassium hydroxide-ethanol solution (56 g/L) weigh 5.6 g of potassium hydroxide, add 10 ml of potassium hydroxide-ethanol solution (10%) to 1 ml. Press to prepare
9.14 High sodium hydroxide solution (10 g/L)
9.15 Sodium hydroxide solution (20%/10%), weigh 20% sodium hydroxide, add water to dissolve and dilute to 10 ml. 9.16 Blue agent: Take 50 mg of p-nitropropene and dissolve it in 50 ml of glacial acetic acid-ethanol solution (20%). 9.17 Methylbenzene standard solution: The H-naphthol product is purified by two times of pure ethanol or the product has a drop point of 12℃~145*:, accurately weigh 50.cmg of methylbenzene refined product. Dissolve in chloroform, transfer to a 100ml volumetric flask, add chloroform to the measured temperature: each milliliter of the solution is equivalent to 2.50mg of methylbenzene
9.18 Methylbenzene standard oil, absorb 1.0ml or 2.0ml of the standard solution, measure 10ml into a 10ml volumetric flask, dilute to the scale with dioxane, this solution is equivalent to 5.0 or 13.0 mg of methylbenzene. 10 Collector
10.1 Spectrophotometer.
10.7 Oil and gas system.
10. 3 Mark the water path disease.
10.4 Vibrating gear machine..
r0.5 Fat extractor.
Centrifuge:
11 Analysis steps
11.1 Grip
11.1.1 Food
GB/T5009.21-2003
The sample is shelled and ground, and filtered through a 2V sieve. Weigh 10.00g of the food sample, cut it into a 150-mm-wide flask, such as 10 sulphuric acid water, and add a spoon, such as 40ml. Methyl chloride, shake it in a multiplier for three times. Soak it overnight with a filter paper. Discard the 2.T~l initial solution, measure the 2℃.m filtrate and place it in a 59mL beaker, add 3 drops of ethylene dichloride, or Hot water is raised and shaken, blood is not present, blow with a suction bulb:
11.t.2 Oil and oil materials
I1.1.2.1 The relatively pure oil: weigh the sample of [.Mr point, use rrt. C to dissolve and wash into 1GM1itT. Transfer the liquid into the bucket.
11.1.2.2 Hand oil: 2,008--5.3 Ya hooked sample, use 40ml right oil aldehyde to dissolve into 100ml. Dispense pain bucket 11.1.2.3 Cottonseed: Test weigh after shelling, crushing, wet hooking. Take 10.00 outside and reduce paper, etc. Put 60mL of fat into the extractor, use 40mL of water to follow the axilization for 8 hours. Transfer the extract into 1cm liquid bucket: 11.1.3. Wash the edible part of vegetables and fruits, dry them, cut them into pieces, and mix them evenly: weigh 25.5g of test tube, add 2g of sodium sulphate solution, grind the milk vigorously until all the tissues are grinded into fine powder, add 10g of anhydrous sodium sulfate and grind it several times until it is completely collected, transfer it to a container, wash the milk with about 5g of anhydrous sodium sulfate, transfer it to a container, grind the milk twice with dioxane, 5g each time, and select the substances sticking to the milk, wash it well and transfer it to a cone-shaped plate, and place it on a container. Hold the heart, 1: 2h, no swimming, use the above-mentioned carrier to leak, and absorb uL filter reduction with 2mL3m tree, and add 3 drops of ethyl acetate in the collection bottle with a dark anti-respiratory device. Steam the liquid on a water bath and discard the methane that evaporates until it is dry, remove the receiving short-term suction bulb and use a short suction bulb to extract the residual agent, 11.2 Purification
11.2.1 Grain
Sound-absorbing steel beaker, make the whole carrier fall completely, draw 1, solid filter, 1 time moving. Put the heavy roasted bucket under the drawer (or oil bottle), spread a piece of light paper, and use a thin layer of about 10% of the selected Jing in the chain as a spare after discarding the six clean drops. Add the test solution into the prepared vertical filter, slowly filter for more than 1 minute, filter, and then add about 2 ml of acetone (1 ml) to clean the inner wall of the beaker. Wash it in the funnel. Soak it for 1 minute to 2 minutes, then drain it. Do this 2 to 3 times. Filter it to 51 ml. Add a small amount of acetone (10 ml) to the end of the filter tube. Wash and dilute it to the dosage in a new dish and mix it: 11.2.2 Oils and oil materials || tt || 11.2.2.1 For relatively clean oils, select a sample containing acetone solution Add 10mL of sodium chlorate to the separatory bucket, shake gently, let stand for 1h, discard the separated layer, put the acetone extract into a commercial centrifuge, centrifuge at 250min for 5h, take the upper clear layer with 1% acetonitrile. Set aside the other separatory bucket, stir for 30min. Take 1% acetonitrile, let stand for 1h, the middle layer with about 10g of anhydrous sodium sulfate, dissolve in 3% diethylene glycol in dioxane, evaporate in anhydrous flask on a vacuum evaporator, discard the separated aqueous layer, and wash with flask once, place in anhydrous magnetic separatory bottle, continue evaporating to the bottom, take out the collection bottle, and use a suction bulb to remove the remaining solvent. Add 3mL of acetone to each bottle, and follow the procedure below. 11.2.2.2 Procedure: In the above petroleum ether extract containing the oil sample, cut 10mL of dimethyl ether into another 4-well tube, shake for 1min, and after separation, shake the petroleum ether layer again with 1mL of dimethyl ether. Combine the two extracts and add 11mL of petroleum aldehyde to wash the extracted dimethyl ether. Add the monomethyl ether layer to 15mL of sodium chloride and 15mL of water, and combine the aqueous layers. Add 25mL of dichloromethane to the dimethyl ether solution four times, each time. Combine the dimethyl ether solution and add 25mL of dichloromethane to the solution. The lack of liquid (208/) with the data twice, to wash away the natural phenolic substances of the inhibitor, then the lacquer liquid, a layer of chloroform and then with sodium flotation (1Ug/L> wash policy: each 5mL, finally with 1mL water wash once. Trichloromethane through anhydrous sodium dehydration station into the collection bottle of the fat extractor. The following 7T, >, "" air two relatively flow of liquid add 3 drops of hexane two end stop liquid. \ \ start to change quickly. 1.2.2.3 Seed: according to the method of 7..2.2, 2 hair cool 174
11.2.3 Phosphorus vegetable. Fruit
GB/T5C09.21-2003
Lead the above Ji Ji extract collection bottle add 31i1., well Rotate the extract in the drop bottle, add 13ml solidifying liquid, rotate the bottle again to make the solidifying liquid fill the inner wall, place 10min. Rotate from time to time: 11.2.1 Connect the suction tube (or filter bottle) to the bottom of the funnel (first copper a piece of filter paper, then needle a 10ml of urine silicone rubber to detect. 12 Determine
absorb .0mT. A standard quick-acting microscope (when 50)4g of the ticket) or mL of the standard stool (equivalent to 1.0g of oral distillation reduction. Connect the test column volume, world ten ml. Burn the Pu, draw 8 diethylene glycol liquid, dissolve in hot water bath, add 3 as the preparation to dissolve, add 15 solidifying light, liquid car, transfer to 25 guest bottles with acetonitrile> wash porcelain detect, select the liquid and put it into the small volume bottle non-vehicle release rate minute, as For comparison with the standard solution, collect the sample and standard solution after the volume adjustment, divide them into ten new test tubes, add 2ml of 2ml of solution (5/1), mix, add 2ml of colorimetric reagent, use a colorimetric cup with water to zero the absorbance at a wavelength of -75mm. At the same time, take two tubes, one of which is the standard solution after the volume adjustment, add 5ml of the sample to the other tube, replace potassium hydroxide with ethanol, and absorb at 475 meters according to the above method, and calculate the results. The sample is 2% in the sample. XA-% obZxz.net
In the formula:
the value of the sample, the unit is g/g; X
A, the reading of the sample without a certain degree of accuracy
the absorbance reading of the blank:
the absorbance reading before the standard drop
the photometric reading of the blank:
the standard sample, the unit is μm (); m——the mass of the sample, the unit is R).
14Precision
Grain sampling 16 : When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed 5% of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed ...The extract was stirred for 1 min, and then separated into two layers. The dimethicone layer was shaken again and the dimethicone layer was washed with 11 ml of petroleum aldehyde. The monomethyl ether layer was added to 15 ml of sodium chloride and water to obtain the juice layer. The dimethyl ether solution was collected with dichloromethane four times, 25 mL each time. The dichloromethane solution was combined. It was collected twice with 5.5 mL of agarose (208/mL) to wash away the phenolic substances in the mixture. Then the solution was washed with dichloromethane and then with sodium iodide (1 μg/L): 5 mL each time. Finally, it was washed once with 1 mL of water. The trichloromethane was passed through an anhydrous sodium dehydration station and poured into the collection bottle of the extractor. After 7 days, 3 drops of hexane were added to the circulating solution. The mixture was replaced quickly. 1.2.2 .3 Seeds: Cool 174% by the method in 7..2.2.2. 11.2.3 Phosphorus vegetables. Fruits. GB/T5C09.21-2003. Add 311% of the extracts in the collection bottle, rotate the bottle to remove the extract, add 13min of solidifying liquid, rotate the collection bottle again to make the solid fill the inner wall, place for 10min. Rotate from time to time: 2 times. Connect the suction tube (or filter bottle) under the funnel according to 11.2.1. First, add a piece of filter paper, then insert a piece of silicone rubber and start to detect. .12 Determine
absorb .0mT. A standard quick-acting mirror (when 50) 4g of the ticket) or mL of the standard stool (equivalent to 1.0g of the oral distillation reduction test column volume, ten ml. burn the park, divide the 8 liquid into diethylene glycol drops, split in a hot water bath, add 3 to dissolve, add 15 tablets to solidify, liquid cart, transfer to a 25%> porcelain bottle with acetone> wash the probe, select the liquid and put it into a small volumetric flask with non-vehicle release rate, as a comparison of the standard muscle liquid, collect the sample and standard after the volume is fixed to 5.CL, make ten new test tubes, add 2m l. Add 2 ml of 5/1.0% of the solution, mix, add 2 ml of colorimetric reagent, use a colorimetric cup with water to zero the absorbance at a wavelength of -75 mm.
At the same time, take two tubes, one of which is a standard tube, add 5 mL of the fixed volume tablet, replace potassium hydroxide with ethanol, and absorb at 475 mm according to the above method. The sample is tested, and the result is calculated. The sample is 2% (XA-% o
In the formula:
the value of the sample, the unit is g/g; X
A, the reading of the sample without a certain degree of accuracy
the absorbance reading of the blank:
the absorbance reading before the standard drop
the photometric reading of the blank:
the standard sample, the unit is μm (); m——the mass of the sample, the unit is R).
14Precision
Grain sampling 16 : When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed 5% of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed ...The extract was stirred for 1 min, and then separated into two layers. The dimethicone layer was shaken again and the dimethicone layer was washed with 11 ml of petroleum aldehyde. The monomethyl ether layer was added to 15 ml of sodium chloride and water to obtain the juice layer. The dimethyl ether solution was collected with dichloromethane four times, 25 mL each time. The dichloromethane solution was combined. It was collected twice with 5.5 mL of agarose (208/mL) to wash away the phenolic substances in the mixture. Then the solution was washed with dichloromethane and then with sodium iodide (1 μg/L): 5 mL each time. Finally, it was washed once with 1 mL of water. The trichloromethane was passed through an anhydrous sodium dehydration station and poured into the collection bottle of the extractor. After 7 days, 3 drops of hexane were added to the circulating solution. The mixture was replaced quickly. 1.2.2 .3 Seeds: Cool 174% by the method in 7..2.2.2. 11.2.3 Phosphorus vegetables. Fruits. GB/T5C09.21-2003. Add 311% of the extracts in the collection bottle, rotate the bottle to remove the extract, add 13min of solidifying liquid, rotate the collection bottle again to make the solid fill the inner wall, place for 10min. Rotate from time to time: 2 times. Connect the suction tube (or filter bottle) under the funnel according to 11.2.1. First, add a piece of filter paper, then insert a piece of silicone rubber and start to detect. .12 Determine
absorb .0mT. A standard quick-acting mirror (when 50) 4g of the ticket) or mL of the standard stool (equivalent to 1.0g of the oral distillation reduction test column volume, ten ml. burn the park, divide the 8 liquid into diethylene glycol drops, split in a hot water bath, add 3 to dissolve, add 15 tablets to solidify, liquid cart, transfer to a 25%> porcelain bottle with acetone> wash the probe, select the liquid and put it into a small volumetric flask with non-vehicle release rate, as a comparison of the standard muscle liquid, collect the sample and standard after the volume is fixed to 5.CL, make ten new test tubes, add 2m l. Add 2 ml of 5/1.0% of the solution, mix, add 2 ml of colorimetric reagent, use a colorimetric cup with water to zero the absorbance at a wavelength of -75 mm.
At the same time, take two tubes, one of which is a standard tube, add 5 mL of the fixed volume tablet, replace potassium hydroxide with ethanol, and absorb at 475 mm according to the above method. The sample is tested, and the result is calculated. The sample is 2% (XA-% o
In the formula:
the value of the sample, the unit is g/g; X
A, the reading of the sample without a certain degree of accuracy
the absorbance reading of the blank:
the absorbance reading before the standard drop
the photometric reading of the blank:
the standard sample, the unit is μm (); m——the mass of the sample, the unit is R).
14Precision
Grain sampling 16 : When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed % of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed 5% of the arithmetic mean; When the absolute difference between two independent determination results under the conditions of quality shall not exceed ...
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.