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GB 29681-2013: Determination of Levamisole residues in milk by High Performance Liquid Chromatographic method
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Determination of Levamisole residues in milk by High Performance Liquid Chromatographic method
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GB 29681-2013
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Basic data | Standard ID | GB 29681-2013 (GB29681-2013) | | Description (Translated English) | Determination of Levamisole residues in milk by High Performance Liquid Chromatographic method | | Sector / Industry | National Standard | | Classification of Chinese Standard | C53 | | Classification of International Standard | 67.020 | | Word Count Estimation | 10,114 | | Quoted Standard | GB/T 6682; GB/T 1.1-2000 | | Adopted Standard | GB/T 6682; GB/T 1.1-2000 | | 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 milk detection sample preparation and high-performance liquid chromatographic method Residues of levamisole. This standard applies to milk detection Levamisole Residues. | GB 29681-2013: Determination of Levamisole residues in milk by High Performance Liquid Chromatographic method
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Determination of Livamisole residues in milk by High Performance Liquid Chromatographic method
National Standards of People's Republic of China
National Food Safety Standard
Determination of Zuo Xuan imidazole residues in milk
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 Zuo Xuan imidazole residues in milk
High performance liquid chromatography
1 Scope
This standard specifies the sample preparation and high performance liquid chromatographic method Residues in Milk levamisole detected.
This standard applies to milk Levamisole Residues.
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
Principle 3
Levamisole remaining in a sample, extracted with ethyl acetate and carbonate buffer solution, C18 column purification, methanol, high performance liquid chromatography
Spectroscopy, 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.
Levamisole hydrochloride 4.1 Standard. Content ≥99.0%.
4.2 methanol.
Anhydrous sodium bicarbonate 4.3. excellent pure.
4.4 sodium carbonate.
4.5 sodium dihydrogen phosphate.
4.6 concentrated ammonia.
4.7 diethylamine. excellent pure.
4.8 acetonitrile.
4.9 phosphoric acid.
4.10 hydrochloric acid.
4.11 C18 solid phase extraction column. 500mg/3mL.
4.12 10% phosphoric acid solution. Take phosphoric acid 70mL, dissolved and diluted with water to 1000mL.
4.13 3mol/L hydrochloric acid solution. Take 250mL of hydrochloric acid, dissolved and diluted with water to 1000mL.
4.14 saturated aqueous sodium bicarbonate. water 1000mL, anhydrous sodium bicarbonate was added to no dissolved, using now.
Saturated aqueous sodium carbonate 4.15. 500 mL water, was added to the sodium carbonate is not dissolved, using now.
4.16 carbonate buffer (about pH = 9). Take a saturated aqueous solution of sodium bicarbonate 900mL, saturated aqueous sodium carbonate was added 100mL, and mix.
4.17 0.02mol/L sodium dihydrogen phosphate buffer solution diethylamine. Take 2.44 g of sodium dihydrogen phosphate, water was added 850mL dissolved, add diethylamine
3mL mixed with 10% phosphoric acid adjusted to pH 7.5, diluted with water to 1000mL.
4.18 1mg/mL levamisole standard stock solution. accurately weighed standard levamisole hydrochloride 10mg, in 10mL volumetric flask, washed with methanol
Dissolved and diluted to the mark, formulated at a concentration of 1mg/mL of stock standard solution levamisole. 2 ℃ ~ 4 ℃ storage period of three months.
4.19 10μg/mL levamisole standard working solution. precise amount of 1mg/mL standard stock solution levamisole 1.0mL, in 100mL
Volumetric flask, dilute to volume with methanol, formulated at a concentration of 10μg L levamisole standard working solution /. 2 ℃ ~ 4 ℃, valid
3 months.
5. Apparatus
5.1 HPLC. with UV detector.
5.2 Analytical balance. a sense of volume 0.00001g.
5.3 Electronic balance. a sense of the amount of 0.01g.
5.4 homogenizer.
5.5 freezing high-speed centrifuge.
5.6 electric heated water bath.
5.7 vortex mixer.
5.8 eggplant-shaped bottle. 50mL.
5.9 centrifuge tube.
5.10 filter. 0.45μm.
Preparation and Storage of sample 6
6.1 Preparation of the sample
An appropriate amount of fresh or frozen or blank test milk, homogeneous mixing.
--- 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
Or less at -20 ℃.
Determination Step 7
7.1 extract
Sample Weigh 5g ± 0.05g, a centrifuge tube, carbonate buffer was added 5mL, ethyl acetate was added 10mL, mix, 6000r/min
Centrifugal 10min, the supernatant was eggplant-shaped flask, together with 10mL ethyl acetate and extracted once, twice combined supernatants rotating at 50 ℃ water bath
Evaporated to dryness, the residue dissolved in carbonate buffer was 5mL standby.
7.2 Purification
3mL C18 column successively with water, methanol and 3mL 3mL activated carbonate buffer, taking stock solution through the column, 3mL water rinsed, dried A
Alcohol 5mL, collecting eluate, dry nitrogen at 50 deg.] C water bath, the residue was dissolved in mobile phase was 1.0mL, membrane filtration, high performance liquid supply
Phase Chromatography.
7.3 Preparation of standard curve
Accurately taken 10μg/mL working standard solution amount levamisole, diluted with mobile phase to prepare a concentration of 10,20,50,100,200,
400 and 800μg/L series of working standard solution for HPLC assay. Peak area was measured to the vertical axis, corresponding to the standard solution
Concentration as the abscissa, the standard curve. Seeking regression equation and correlation coefficient.
7.4 Determination
7.4.1 LC Conditions
7.4.1.1 Column. C18 (l50mm × 4.6mm, particle size 5μm), or equivalent person.
7.4.1.2 Mobile phase. 0.02mol/L sodium dihydrogen phosphate buffer solution of diethylamine in methanol (70 30, volume ratio).
7.4.1.3 flow rate. 1mL/min.
7.4.1.4 Detection wavelength. 220nm.
7.4.1.5 Injection volume. 50μL.
7.4.1.6 Column temperature. 30 ℃.
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
Liquid levamisole response value should be within the linear range of the detection 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.
Calculation and Expression of Results 8
Residue (μg/kg) in a sample according to the class of levamisole formula (1).
X = A × cS × VAS × m
(1)
Where.
--- for X-try levamisole feed residues, micrograms per kilogram (μg/kg);
A --- peak area of sample solution levamisole;
cS --- standard working solution concentration of levamisole, micrograms per liter (μg/L);
V --- The residue was dissolved in mobile phase volume in milliliters (mL);
--- the AS standard working solution of the peak area of levamisole;
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 detection sensitivity, accuracy and precision
9.1 Sensitivity
The detection limit of the method was 2.5μg/kg, the limit of quantitation of 5μg/kg.
9.2 Accuracy
This method of adding 5μg/kg ~ 20μg/kg on recovery levels of 70% to 110%.
9.3 Precision
The relative standard deviation of the method ≤20%, inter-assay relative standard deviation ≤20%.
Appendix A
Chromatogram
Figure A.1 levamisole chromatogram standard solution (20μg/L)
Figure A.2 milk blank sample chromatogram
Figure A.3 milk sample blank add levamisole chromatogram (20μg/kg)
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