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GB 29702-2013: Determination of Trimethoprim residues in aquatic products by High Performance Liquid Chromatographic method
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Determination of Trimethoprim residues in aquatic products by High Performance Liquid Chromatographic method
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GB 29702-2013
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Basic data
| Standard ID | GB 29702-2013 (GB29702-2013) |
| Description (Translated English) | Determination of Trimethoprim residues in aquatic products by High Performance Liquid Chromatographic method |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | C53 |
| Classification of International Standard | 67.020 |
| Word Count Estimation | 10,174 |
| Quoted Standard | GB/T 6682; GB/T 1.1-2000 |
| Adopted Standard | GB/T 6682; GB/T 1.1-2000; SC/T 3016 |
| Regulation (derived from) | China Food & Drug Administration [2013] No. 234, November, 1, 2013 |
| Issuing agency(ies) | Ministry of Agriculture of the People's Republic of China, National Health and Family Planning Commission of the People's Republic of China |
| Summary | This standard specifies the Aquatic trimethoprim residual amount sample preparation, high-performance liquid chromatographic method. |
GB 29702-2013: Determination of Trimethoprim residues in aquatic products by High Performance Liquid Chromatographic method
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Determination of Trimethoprim residues in aquatic products by High Performance Liquid Chromatographic method
National Standards of People's Republic of China
National Food Safety Standard
Determination of trimethoprim residues in aquatic piperidine
High performance liquid chromatography
Published 2013-09-16
2014-01-01 implementation
Ministry of Agriculture, People's Republic of China
National Health and Family Planning Commission People's Republic of China released
National Food Safety Standard
Determination of trimethoprim residues in aquatic piperidine
High performance liquid chromatography
1 Scope
This standard specifies the sample preparation and high performance liquid chromatographic method trimethoprim residues in aquatic products.
This standard applies to fish (including eel), shrimp, crab and turtles Residues in edible tissues of trimethoprim.
2 Normative references
The following documents for the application of this document is essential. For dated references, only applies to the version dated paper
Pieces. For undated references, the latest edition (including any amendments) applies to this document.
GB/T 6682 Water for analytical laboratory specifications and test methods
SC/T 3016 aquatic sampling
Principle 3
The specimens remaining trimethoprim, extracted with chloroform and an acidic methanol solution, back extracted with methylene chloride, the net MCX SPE
Of HPLC - UV determination, external standard.
4 Reagents and materials
The following reagents used, unless otherwise stated were of analytical reagent; water as a water line with GB/T 6682 provisions.
Trimethoprim 4.1 Standard. content ≥98%.
4.2 chloroform. HPLC grade.
4.3 Methanol. HPLC grade.
4.4 perchloric acid. pure class distinctions.
4.5 Sulfuric acid. excellent pure.
4.6 dichloromethane. chromatography.
4.7 Sodium hydroxide. pure class.
4.8 acetic acid. excellent pure.
4.9 ammonia.
4.10 MCX cation SPE. 60mg/3mL, or equivalent person.
4.11 0.5% perchloric acid solution. Take perchlorate 5mL, dissolved and diluted with water to 1000mL.
4.12 0.1moL/L sulfuric acid solution. Take 5.4mL of sulfuric acid, dissolved and diluted to 1000mL with water.
4.13 2moL/L Potassium hydroxide. potassium hydroxide to take 112.2g, dissolved and diluted with water to 1000mL.
4.14 5% acetic acid solution. Take 50mL acetic acid, dissolved and diluted with water to 1000mL.
4.15 5% ammonia in methanol. aqueous ammonia to take 5mL, dissolved in methanol and diluted with 100mL.
4.16 100μg/mL trimethoprim standard stock solution. Weigh accurately trimethoprim standard 10mg, in 100mL flask with methanol
Dissolved and diluted to the mark to prepare a stock standard solution trimethoprim concentration of 100μg/mL of. -4 ℃ or less from light, valid for 3
Months.
4.17 10μg/mL trimethoprim standard working solution. precise amount of trimethoprim 1.0 mL standard stock solution, to a 10mL volumetric flask, with methyl
Alcohol diluted to the mark, formulated at a concentration of trimethoprim working standard solution 10μg/mL of. -4 ℃ or less from light, valid for 3
Months.
5 Apparatus
5.1 HPLC. with UV detector.
5.2 Analytical balance. a sense of volume 0.00001g.
5.3 Balance. a sense of the amount of 0.01g.
5.4 homogenizer.
5.5 vortex mixer.
5.6 centrifuge.
5.7 rotary evaporator.
5.8 SPE.
5.9 eggplant-shaped bottle.
5.10 stoppered centrifuge tube. 50mL.
5.11 separatory funnel. 150mL.
5.12 filter. 0.45μm.
Preparation and Storage of sample 6
6.1 Preparation of the sample
Fresh or thawed take appropriate blank or test tissue, minced, and homogenized.
--- the test sample taken after homogenization, as the feed try.
--- blank sample taken after homogenization, as a blank sample.
--- blank sample taken after homogenization, adding a suitable concentration of the standard working solution, is added as a blank sample.
Save 6.2 sample
-18 ℃ below saved.
Determination Step 7
7.1 extract
Sample Weigh 5g ± 0.05g, in 50mL stoppered centrifuge tube, add chloroform 15mL, methanol 14mL, 0.1mol/L sulfuric acid solution
Solution 6mL, vortexed 2min, 4000r/min centrifugal 3min, 150mL supernatant to a separatory funnel. Methanol was added to the residue
And 14mL 0.1mol/L sulfuric acid solution, 6 mL, extraction was repeated once, the two supernatants were combined in a separatory funnel, was added 2mol/L hydroxide
Solution of potassium 2mL, dichloromethane 30mL, shake for 2min, standing layer, the lower layer was taken to the eggplant-shaped flask, added to a separatory funnel with dichloromethane
30mL extraction was repeated once, the lower two combined solution at 40 ℃ rotary evaporated to near dryness, washed with 5% acetic acid solution to dissolve the residue 6mL,
spare.
7.2 Purification
MCX cation exchange column washed with methanol and 5% acetic acid solution 6mL 6mL activated, taking stock solution passed through the column, washed with 5% acetic acid solution
And 6mL 6mL methanol, and eluted with ammonia in methanol 15mL, at 40 ℃ rotary evaporated to near dryness and dissolved with mobile phase 1.0mL
The residue was filtered through a filter for the Determination.
7.3 Preparation of standard curve
The precise amount of trimethoprim working standard solution amount, diluted with mobile phase to prepare a concentration of 50,200,500,1000,2000,
5000μg/L standard solutions for HPLC assay. To measure peak area for the vertical axis, corresponding to the concentration of standard solution of abscissas
Standard, the standard curve. Seeking regression equation and correlation coefficient.
7.4 Determination
7.4.1 Chromatographic conditions
7.4.1.1 Column. ZORBAX-C18 column (4.6mm, particle size 5μm 250mm ×), or equivalent person.
7.4.1.2 Mobile phase. 0.5% perchloric acid methanol solution (30 70, volume ratio).
7.4.1.3 flow rate. 1.0mL/min.
7.4.1.4 Column temperature. 35 ℃.
7.4.1.5 Injection volume. 20μL.
7.4.1.6 Detection wavelength. 230nm.
7.4.2 Assay
Take a sample solution and standard solutions corresponding, for single or multi-point calibration, by external standard method, the peak area is calculated. Standard solution and sample solution
Trimethoprim response was linear within the range of values to be detected by the instrument. In the chromatographic conditions, sample was added standard solution and blank solution
HPLC liquid in Appendix A. FIG.
7.5 Blank test
But without addition of the sample, the same steps employed in parallel operation.
8 results calculated
Residues in the specimens trimethoprim (μg/kg) according to formula (1).
X =
c × V
(1)
Where.
--- for X-try feed residues trimethoprim micrograms per kilogram (μg/kg);
--- C concentration in the sample solution trimethoprim, in micrograms per milliliter (μg/mL);
The residue was dissolved V --- volume in milliliters (mL);
m --- try supply feed mass in grams (g).
Note. The blank value should be subtracted from the results, expressed as the arithmetic mean of the measurement result measured parallel to three significant figures.
9 The method of sensitivity, accuracy and precision
9.1 Sensitivity
The limit of quantification was 20μg/kg.
9.2 Accuracy
This method of adding 20μg/kg ~ 1000μg/kg on recovery levels of 70% to 110%.
9.3 precision of the method
≤15% relative standard deviation in this method and inter - batch relative standard deviation of ≤15%.
Appendix A
Chromatogram
Figure A.1 trimethoprim chromatogram of the standard solution (200μg/kg)
Figure A.2 in Muscle tissue sample blank chromatogram
Figure A.3 in Muscle tissue sample blank add chromatogram trimethoprim (200μg/kg)
T/B
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