GB/T 5009.172-2003 Determination of trifluralin residues in soybeans, peanuts, soybean oil and peanut oil

This standard specifies the method for determining the residual amount of trifluralin in soybean, peanut, soybean oil and peanut oil. This standard is applicable to the determination of the residual amount of trifluralin in soybean, peanut, soybean oil and peanut oil. The detection limit of this method is 0.001ng. The detection range is 0.01μg/mL～0.10μg/mL. GB/T 5009.172-2003 Determination of the residual amount of trifluralin in soybean, peanut, soybean oil and peanut oil GB/T5009.172-2003 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
GB/T 5009.172--2003
Determination of trieluralin residues insoybean peanul , soybean oil, peanut oil. 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
This standard was issued by the Ministry of Health of the People's Republic of China and is under the jurisdiction of the drafting unit of this standard. The main drafters of this standard are Hai Shili and Chan Xiusa. GB/T5009.172-2003
GD/T 5009.172—2003
Trirlrulim, also known as trichlorfon, trichlorfon and trichlorfon. It is a low-toxic weed killer. China has formulated its own limit of trichlorfon residues in soybean, peanut, soybean oil and peanut oil. The limit of trichlorfon residues in soybean, peanut, soybean oil and peanut oil is 0.05kg. This standard is applicable to the determination of trichlorfon residues in soybean, peanut, soybean oil and peanut oil that have been treated with trichlorfon preparations. Scope
Determination of trichlorfon residues in soybean, peanut, soybean oil and peanut oil. This standard specifies the determination method of trichlorfon residues in soybean, peanut, soybean oil and peanut oil. This method is applicable to the determination of fluroxypyrimidine residues in soybean, peanut, soy milk and peanut oil. The detection limit of this method is 0.001tg: Linear model: 0.C)pg/ml.-0.1cg/mL2 Principle
CB/T5009.172-2003
The fluroxypyrimidine in the sample is extracted with methanol and acetone. After liquid-liquid distribution and Florisil column purification, it is determined by gas chromatography with an electric detector. Quantitative analysis by external standard method.
3 Experimental results
3.1° Methanol: reheated in a all-glass thermostat
3.2 Acetone, reheated in a all-glass thermostat.
3.3 Stone pool: Take 10mL of cellulose (6℃) and add sodium iodide and 1% sodium hydroxide: cool for 1-8 minutes, then steam and adjust the mixture.
3.4 ​​Anhydrous sodium pyrolysis Take 50g of anhydrous sodium pyrolysis and filter it with 50mL of silica gel. Add 25mL of non-aluminum aldehyde to filter it. Bake at 350℃ for 4h after natural wind. Put it in a desiccator for later use. 3.5 Anti-sodium pyrolysis solution 50R/L
9.6 Take the sample and layer it (50 days to 12 days) and burn it at 650℃ for 6h: dry it and add 5% (mass fraction) hot water to make a slice and shake it evenly, then put it in a desiccator for later use.
3.7 Degreased ladder: Put the degreased ladder into the extractor in the required area, add acetone-petroleum aldehyde (1-%) as solvent, reflux on a water bath for 1 hour, and then evaporate to 10% by weight.
3.B Activated carbon: Use 1008mol/L of activated carbon to make it into a state, boil it for 10 min, then filter it, wash it with hot water to remove chloride ions, dry it at 120°C, and use
3.9 Chlorhexidine standard solution: Use petroleum ether, trilurim standard (containing 99.5% Trilurim) to prepare 1.0ug/mL of chloramine solution, prepare it for filtration, select 10% hydroxyethyl ether before use, and use the standard working conditions as 4.1 Relevant collector: Electrocardiogram capture detector (ECD, Ni\) 4.2 Electric crusher:
4.3 Electric heat collector
4.4 Heart machine: 3 0(heart/i.
All my glass steam package
Rotate and expose naturally.
4.7 Chromatography: Put 1.5cm long 25m glass room into the flask. 4.8 One corner flask: 255 ml
4.9 Divide the sample into 125mL, 250ml
GU/50C3,172—2003
S Analysis steps
5.1 Sample 1.0kg is weighed and 1608 portions are taken by electric machine according to the quartering method. Then, 40 portions of soybean oil and peanut oil are prepared.bzxZ.net
5.2.1 Soybean and peanut
Take 10.0g of peanut sample and add 100m of tea to 250ml. Add 100m of tea to the separatory funnel and vibrate for 30min. After filtering, add 1Cmin. Pipette 24mL of the filtrate to 252 and add 1 00mT monosodium iodide. Add 50ml, shake the stone and take 2min, let it stand for stratification, then put the lower layer into another full bucket and take 50mL of stone again. Boil water at 259℃ in a 6-bowl anhydrous acid-free funnel, and evaporation in a water bath until it is purified. 5.2.2 Soybean oil and peanut oil
weigh soybean oil or peanut oil 5.08, shake 0mL acetone and add 125mL, separate the liquid into a bucket, add 10ml of water, shake for 1min, let it stand for stratification, separate the oil layer into two buckets, add 5nml of acetone and 1gmE of water until it is repeated, remove, combine the water and emulsify the serious centrifugation to remove the source, and absorb 24mL into a 250mL separatory. In the leak, 100% of the solution fell into the mixture. 5.1 "Self-secreting aldehyde source" method 5.3 Purification
Column chromatography Note: Use a little cotton wool to pad the bottom, add 1cm of anhydrous sulfuric acid, mix 5R with silica gel, 0.1g of active ingredients, 0.1-cm high anhydrous sodium sulfate, discard the product ml of petroleum fermentation pre-rinse, transfer the root glass to the column, open the lower end of the column to collect the clear outflow in a 3501L round-bottom flask, when the anhydrous sulfuric acid is completely removed, use a 1um stone pool at ml./minml/in to wash the bottom. Transfer the washed filter with a 1.0m filter to a 0-0 volumetric bottle, observe the oil aldehyde fraction and then determine the concentration. 5.4 Color filling reference conditions||tt ||Chromatographic column: inner diameter %m2m, filled with 4.5%2002.%(V-12) Chrono3orhWAw-DMCS phase;
column short, 19
injection density: 250 yuan
instrument flow rate, 250?
carrier gas: (9.0 mL/min)
5.5 determination rate
use standard T as liquid oil screen into D.0C.0.01.0.02.0.04, 0.55.D.CK.0.10R/mI. Take 1.1 respectively, inject rod, repeat each time 3 times, record the usage time. Pair the peak area with the value of chloroform content to find the linear regression line. At the same time, inject the purified sample into the chromatograph. Substitute the obtained peak height or peak area into the equation to calculate the amount of chloramine in the sample. Under the high-speed chromatography, the retention rate of chloramine is 2mn5, and the result is calculated by the following formula:
XEXVX5
Where:
X--the residual amount of chloramine in the sample, unit is microgram per gram (mg/kg); ... the content of chloramine in the sample, unit is microgram per liter (μg/L); --the final fixed volume, unit is liter (): 22
Two sample volumes, unit is g ()
5.-Dilution factor of the sample,
The result is calculated with retaining significant figures.
E Precision Width
GB/T 5009,172—2003
The difference between the previous independent determination results obtained under repeated conditions shall not exceed the arithmetic half-mean. The color tone diagram
Color tone diagram
Steaming Ling
Figure 1 Chromatogram of Baoqiuling Standard
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