This standard specifies the method for the determination of phoxim residues in cereals, vegetables and fruits. This standard is applicable to the determination of phoxim pesticide residues in cereals, vegetables and fruits. The detection limit of this standard is 0.01 mg/kg. GB/T 5009.102-2003 Determination of phoxim pesticide residues in plant foods GB/T5009.102-2003 Standard download decompression password: www.bzxz.net

18 67,040
National Standard of the People's Republic of China
GB/T5009.102—2003
H14875—1!94
Determinatiun of phuxim eslicide pesticide residues in plant-derived foods Residues in vegetable foods
Issued on August 11, 2003
Ministry of Health of the People's Republic of China
China National Standardization Supervision Committee
Implementation on January 1, 2004
CAT500a.1042003
This standard is based on GB/T 14875-1994 for the determination of pungent pesticide residues in vegetable foods. The main differences between this standard and GB14875-1991 are as follows: The Chinese name of the standard has been modified. The Chinese name of the standard has been changed to Determination of pungent and phosphorus pesticide residues in vegetable foods: --- It was compiled in accordance with GB/T 20007.4-200C1&.
This standard is based on the requirements of the Ministry of Health of the People's Republic of China. Section 4: Chemical analysis methods > The structure of the original standard is revised. The units of this standard are: Food Hygiene Supervision and Inspection Institute of the Ministry of Health, Institute of Natural Resources Research of Xinjiang Academy of Agricultural Sciences, Beijing Agricultural University, Institute of Energy Application of Xinjiang Academy of Agricultural Sciences. The main drafters of this standard are: Shen Zaihuan and Zhang Linfu. The original standard was revised in 1991 and this is the first revision. tScope
GB/T $009.102—2003
Determination of pungent pesticide residues in plant foods This standard specifies the method for determining pungent carbon and phosphorus residues in vegetables, fruits and vegetables. This standard is applicable to the determination of octinoxate pesticides in water. The detection limit of this standard is 2.01 me/g. The sample containing organic matter is burned in a hydrogen-rich atmosphere and emits characteristic light in the form of HPC fragments. This characteristic light is received by a photomultiplier tube through a film, converted into an electric signal, and then a micro-current amplifier is used to record the standard and sample's high and low values ​​respectively. The content of these substances or samples can be detected by other methods. 3.1. Carboxylic acid.
3.2 Avoid.
3.3 No water.
3.4 ​​Activated carbon: Soak in 3 mol/1 salt overnight, filter and wash with neutral water, and dry at 129°C for use. 3.5 Standards
3.5.1 Magnetic phosphorus (Xm, 90%,
3.5.2 Preparation of standard solution: Weigh the standard sulfur sample and prepare it in a 1mg/ml standard container.
4.1 Gas chromatography, flame chromatograph. 4. 2 Electric drug collector.
4.3 KL liquid compressor.
4.4 Extractor.
4.5 Sieve bottle.350 total 1.
4.6 Divided by sieve bucket + 20mI.
5 Sample preparation
Dare to use drug sample, crush it with crusher - after 2 days of sieve, make the sample. Take vegetable and fruit samples, discard the non-edible ones. After the crushed effect is broken, the vegetable or fruit samples will be crushed. The steps of analysis
6.1 6.1.1 Weigh 30 g of each grain sample accurately, put it into a 100 mL cork bottle, add 50 mL of petroleum ether, filter, wash once with 10 mL of oil-free filter, combine the filtrate, pass through anhydrous sodium sulfate, and use a K-D concentrator to reduce the volume to 80%, and distribute it in a color-coded manner. 6.1.2 Add 50 mL of blue rack sample to a volume of 0.301 g, and place it in a vertical plate. Use a stone injection to make it deep. 5009.302—2003
1Cml Ricoh short extraction for 12h, then add 1g--3g (root hot dish color home plate) required carbon quick recommendation 0.55 let stand for 5min, add ice, thin and then use 50ml. acetone wash liquid to enter 100mt.2 sodium sulfate water paint solution, use 151mL petroleum sulphate to extract twice, add benzene to take liquid, get the product and adjust the volume to 10mL. Wait for gas rejection and color analysis. 6.1.3 Fruit: Weigh 25g of fruit sample, add 1.5g of active Carbon monoxide is used to push the sample, and the sample is wrapped with a shrink wrapper, placed in a tester, and 12L of petroleum aldehyde-lactone (1 + 1) is added. After a period of exposure to light, it is refrigerated at 6u℃ for 4 hours, 4-5 times per hour, and then added to the separatory bucket, and 30mL of sodium sulfate aqueous solution is added to separate the stone layer. The water layer is extracted with 20ml of benzene, and the oil aldehyde is removed once, and the oil aldehyde is passed through anhydrous sodium carbonate, and the petroleum ether layer is condensed to 5L: wait for gas chromatography analysis. 6.2 Gas chromatographic analysis
6. 2.1 Gas chromatography conditions
5.2.1.1 Chromatographic column, inner diameter 3mm, length 1m, equipped with OV-101/ChramnrhW.AW.[3MCs8c日--100日.
6.2.1.2 Gas flow rate, carrier gas (N, 180ml./min, air 60mL/miu, hydrogen 6lmL/min6.2.1.3 Temperature temperature = 5, injection 185℃, detector 250℃, 6.2.2 6.2.2 Qualitative analysis: qualitative analysis is carried out by breaking the retention time of the standard. 6.2.2.2 Quantitative analysis: quantitative analysis is carried out by external standard method.
Result calculation
Calculate according to the following formula:
Wherein;
the content of chlorpyrifos in the sample, in mg/isg; F
the amount of standard chlorpyrifos in the sample, in nanogram (ton); F
the volume of the standard sample after injection, in nanogram (ton); ---the peak height of the standard sample, in millimeter (m); f
the quotient of the sample, in millimeter (mm); the mass of the sample: in gram (g)
The calculation result shall retain all significant figures.
8 Precision block
Under the condition of using gram, the absolute value of the two independent determination results shall not exceed 10% of the arithmetic mean value, 9 Chromatographic surface of phoxim agricultural products
Xeno used the chart,
2,bzxZ.net
: The mountain time of the brand standard product of the company is 4.33m. Figure
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