This standard specifies the determination of tricyclazole residues in rice. This standard is applicable to the determination of tricyclazole residues in rice. The detection limit of this standard is 10ng. GB/T 5009.115-2003 Determination of tricyclazole residues in rice GB/T5009.115-2003 Standard download decompression password: www.bzxz.net

ICS 67. 343
National Standard of the People's Republic of China
GB/T 5009.115—2003
Replaces GB/T14929.a—1994
Determination of tricvelazole residues in rice
Determination of tricvelazole residues in riceIssued on August 11, 2003
Ministry of Health of the People's Republic of China
National Standardization Administration
Implementation on January 1, 2004
CB/T 5009.115—2003
This standard replaces GB/T14929.9—1994 "Determination of tricvelazole residues in rice". Compared with GB/T14929.9-1994, the main revisions of this standard are as follows: Modification of the Chinese names of the standards, the Chinese name of the standard is changed to Determination of tricyclazole retention in valleys. --- According to the GB/T20001.4·20014 cup standard writing rules Part 4: Chemical analysis method 3, the results of the original standard were analyzed,
This international annotation was proposed by the Chinese People's Government and the Ministry of Health of the People's Republic of China. The originating units of this standard are: Zhejiang Medical College, Zhejiang Provincial Agricultural University, China National Rice Research Institute: This standard was first issued in 1994, and this is the second revision.
1 Scope
Determination of tricyclazole residues in rice
This standard specifies the determination of tricyclazole residues in rice. This standard is used for the determination of tricyclazole residues in rice. The test volume of this standard is 10g.
2 Principle
GB/T 5009.115—2003
Monocyclazole was extracted by organic extraction and purified and then collected by gas chromatography-mass spectrometry with a gas phase detector and compared with the standard. 3.1 Gas phase amplification instrument with a gas phase detector: 3.2 Small electric pulverizer,
3.3 Rotary evaporator:
25cm Soxhlet extractor.
50W electric heating mantle.
Fully glass thermal stack apparatus
Carbon glass chromatography, 1.=cm (inner diameter) × 25cm3.8 Small electric evaporator.
| Reagents
Ethyl alcohol (heavy alcohol)
Methanol (egg alcohol).
4. Internal ()
4.5 Neutral oxidation group 10c day--299 day (430℃ activation 6h, used for 130℃ drying 4h, add R% water to deactivate 4.6 Acid-free sodium (15u drying 4h).
9. A% tricyclic seat (tricyclaole) standard 5 Analysis steps
5.1 Extraction and purification
5.1.1 Sample (.m 258, shell 12.5g, respectively, with filter paper packaging effect of the case of the extractor , add 100:1 ethyl acetate and soak overnight, extract for 6 hours. Take the product and transfer it to the concentration bottle through anhydrous sodium sulfate, and rotate for nearly ten minutes. 5.1.2 Purification
Explosion chromatography: Load the following groups of glass from top to bottom, 2cm anhydrous dead acid, 10g neutral alumina, 2cm sodium sulfate, first rinse with 25ml of monoxide, then transfer to the concentration bottle with 25ml of dichloromethane, add 20ml, 20mL of dichloromethane to rinse, remove the elution agent, and finally add dichloromethane-methanol (6-!) to rinse, collect the elution, concentrate, rotary evaporate, 5.2.1 Chromosorb WHPso-lus carrier with 1% PEC in glass: 4mm (outer diameter>×100mm). GB/T5009.115—2003 5.2.2 Temperature: temperature 228℃, vaporization temperature 245, detection room 205.2.3 Air flow: oxygen 57mL/min, hydrogen 8mL/min, gas 120mLmin5.2.4 Paper speed: 4 mtr./min: 5.2.5 Retention time: under the above conditions, the retention time of tricyclazole is 7min36s. 5.3 Determination: Use external standard method to prepare a series of tricyclazole standard curves first, so that the response of static is in a relationship. Standard solution: Carefully weigh 22% of tricyclazole standard and prepare it into 210-g/mL solution with propane. Find the recovery range of the sample content suitable for the sample, measure the peak heights of tricyclazole standards with different concentrations, and at the same time add the sample (with the same injection volume as the standard) into the gas chromatograph. Compare the obtained peak height with the similar peak height of the standard, and record the tricyclazole content in the sample. 6 Calculation of the viscosityWww.bzxZ.net
The following formula is used for calculation:
Where,
-the content of tricyclazole in the sample, in milligrams per kilogram (mg/kg);-the peak height of the sample, in millimeters (mm);-the peak height of the standard, in millimeters (tm); A-the content of tricyclazole in the standard sample, in nanograms (ng);-the volume of acetone, in milliliters (mL);,
the volume of the sample, in microliters (L); the mass of the test sample, in grams. g! .
The calculation shall be carried out using valid digits,
7 The absolute difference of the results of the three independent determinations obtained under the conditions of precision shall not exceed 1% of the arithmetic mean value. 8 Other
The content of tricyclazole in the standard sample and the standard cyproconazole must be calculated! A standard tricyclazole
a standard tricyclazole in a tube,
Figure! Tricyclazole also spectrum
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.