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GB 29706-2013: Determination of Dapsone residues in animal derived food by Liquid Chromatography-tandem Mass Spectrometric method
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Determination of Dapsone residues in animal derived food by Liquid Chromatography-tandem Mass Spectrometric method
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GB 29706-2013
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Basic data
| Standard ID | GB 29706-2013 (GB29706-2013) |
| Description (Translated English) | Determination of Dapsone residues in animal derived food by Liquid Chromatography-tandem Mass Spectrometric method |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | C53 |
| Classification of International Standard | 67.020 |
| Word Count Estimation | 10,132 |
| 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 animal-derived food dapsone residue detection sample preparation and liquid chromatography tandem mass spectrometry. |
GB 29706-2013: Determination of Dapsone residues in animal derived food by Liquid Chromatography-tandem Mass Spectrometric method
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Determination of Dapsone residues in animal derived food by Liquid Chromatography-tandem Mass Spectrometric method
National Standards of People's Republic of China
National Food Safety Standard
Determination of dapsone residues in animal foods
Liquid chromatography - tandem mass spectrometry
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 dapsone residues in animal foods
Liquid chromatography - tandem mass spectrometry
1 Scope
This standard specifies the animal food dapsone Residues sample preparation and liquid chromatography - tandem mass spectrometry.
Residues in muscle and liver tissue dapsone is applicable to the porcine and bovine.
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.
Specifications and test methods for laboratory water GB/T 6682 analysis.
Principle 3
Dapsone remaining in a sample, extracted with acetonitrile, hexane degreasing, MCX, purified by liquid chromatography - tandem mass spectrometry, the external standard method
Quantitative.
4 Reagents and materials
The following reagents used, unless otherwise stated are analytical reagents, water as a water line with GB/T 6682 provisions.
4.1 dapsone Standard. Content ≥98%.
4.2 Acetonitrile. chromatographically pure.
4.3 n-hexane.
4.4 concentrated ammonia.
4.5 hydrochloric acid.
4.6 MCX SPE. 60mg/3mL, or equivalent person.
4.7 1mol/L hydrochloric acid solution. Take 8.4mL of concentrated hydrochloric acid was dissolved and diluted to 100mL with water.
4.8 0.1mol/L hydrochloric acid solution. 0.84mL take concentrated hydrochloric acid, dissolve and dilute to 100mL with water.
4.9 5mmol/L ammonium acetate solution. Take 0.385 g ammonium acetate, dissolved and diluted to 1000mL with water, membrane filtration.
4.10 5% ammoniated acetonitrile. concentrated aqueous ammonia Take 5mL, dissolved in acetonitrile and diluted to 100mL.
4.11 1mg/mL dapsone standard stock solution. Weigh accurately dapsone 10mg, in 10mL volumetric flask, dissolved in methanol and diluted to the mark with
Degree, formulated as dapsone stock standard solution at a concentration of 1mg/mL of. -20 ℃ dark preservation, valid for six months.
4.12 10μg/mL dapsone standard working solution. precise amount of 1mg/mL standard stock solution 0.1 mL dapsone, in 10mL volumetric flask,
Dilute with methanol, formulated as dapsone standard working concentration of 10μg/mL of. -20 ℃ dark preservation, valid for six months.
4.13 100ng/mL dapsone standard working solution. precise amount of 10μg/mL dapsone working standard solution 0.1mL, in 10mL volumetric flask
, Diluted with methanol to scale, formulated at a concentration of 100ng/mL dapsone the standard working solution. -20 ℃ from light, valid
6 months.
5. Apparatus
5.1 liquid chromatography - tandem mass spectrometry. equipped with an ESI source.
5.2 Analytical balance. a sense of volume 0.00001g.
5.3 Balance. a sense of the amount of 0.01g.
5.4 centrifuge.
5.5 nitrogen blow device.
5.6 vortex mixer.
5.7 SPE.
5.8 ultrasonic cleaning machine.
5.9 homogenizer.
5.10 filter. 0.22μm.
5.11 centrifuge tube. 50mL.
Preparation and Storage of sample 6
6.1 Preparation of the sample
Fresh or frozen 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
Or less at -20 ℃.
Determination Step 7
7.1 extract
Sample Weigh 2g ± 0.05g, a centrifuge tube, acetonitrile was added 10mL, vortexed 2min, n-hexane was added 5mL, vortexed
1min, ultrasonic 5min, 5000r/min centrifugal 10min, discard the upper layer of n-hexane solution. Acetonitrile was taken to another centrifuge tube, was added 1mol/L
Hydrochloric acid solution 10mL, Vortex, spare.
7.2 Purification
MCX column washed with 5mL methanol and 5mL water activation, taking stock solution through the column, controlling the flow rate of less than 1mL/min, with 0.1mol/L
5mL methanol and 5mL solution of hydrochloric acid rinsed, drained, eluting with 5% ammoniated 5mL acetonitrile, dry nitrogen at 40 ℃ water bath, mobile phase
The residue was dissolved 1.0mL, Vortex for liquid chromatography - tandem mass spectrometry.
7.3 Preparation of standard curve
The precise amount of 100ng/mL working standard solution amount dapsone, diluted with methanol, concentrations were formulated and 0.5,1,2,5,10
20μg/L standard solution series. For liquid chromatography - tandem mass spectrometry. A characteristic ion mass chromatogram peak area for the vertical axis, control 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 (150mm × 2.1mm, particle size 5μm), or equivalent person.
7.4.1.2 mobile phase. acetonitrile 5mmol/L ammonium acetate (50 50, volume ratio).
7.4.1.3 Column temperature. 40 ℃.
7.4.1.4 Injection volume. 20μL.
7.4.2 MS conditions
7.4.2.1 Ion Source. ESI source.
7.4.2.2 Scan mode. positive ion scan.
7.4.2.3 Detection mode. selective reaction monitoring.
7.4.2.4 Spray voltage. 4800V.
7.4.2.5 Ion transfer tube temperature. 350 ℃.
7.4.2.6 Sheath Gas Pressure. 40arb.
7.4.2.7 Auxiliary gas pressure. 5arb.
7.4.2.8 dapsone optimization parameters selected reaction monitoring. Table 1.
Table 1 dapsone selected reaction monitoring of optimization parameters
Drug Name qualitative and quantitative ion ion pair
Collision energy
eV
Dapsone
249.0 > 108.1
249.0 > 92.2
249.0 > 108.1 21
twenty three
7.4.3 Determination
7.4.3.1 qualitative determination
By retention time of sample chromatogram with retention times of the respective standards, wherein each of the ion peaks and the corresponding concentration of the standard
Wherein each of the ion peaks qualitative contrast. Sample and standard deviation of the relative retention time of not more than 5%; with a sample wherein ions
Consistent with the abundance relative abundance fairly mixed standard solution concentration, relative abundance does not exceed a predetermined deviation Table 2, the sample can be stored is determined
The respective analyte.
The maximum allowable deviation relative ion abundance qualitative determination of Table 2
The relative ion abundances > 50 20 ~ 50 10 ~ 20 ≤10
Permissible relative deviation ± 20 ± 25 ± 30 ± 50
Ratio for the sample and standard solutions try quantitative ion area of single-point calibration for quantification.
7.4.3.2 quantitative determination
Take a sample and standard solutions, by external standard method, in order to quantify the peak area, the standard solution and the sample solution response value should be at dapsone
The linear range of the detection equipment. In the above-described chromatography - mass spectrometry under conditions dapsone standard solution, the tissue sample and the blank sample blank add organizations
The ion mass chromatogram of the sample solution in Appendix A.
7.5 Blank test
But without addition of the sample, the same steps employed in parallel operation.
Calculation and Expression of Results 8
The residual amount of ammonia present the sample of the sulfone (μg/kg) according to formula (1).
X =
A × cS × V
AS × m
(1)
Where.
--- try feed for X-sulfone remaining amount of ammonia present in units of micrograms per kilogram (μg/kg);
A --- peak area of sample solution of ammonia present sulfone;
cS sulfone --- ammonia concentration present in the standard working solution, in micrograms per liter (μg/L);
V --- The residue was dissolved with the volume of mobile phase, milliliters (mL);
--- the AS standard working solution of ammonia present peak area sulfone;
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 0.1μg/kg, the limit of quantitation was 0.5μg/kg.
9.2 Accuracy
This method of adding 0.5μg/kg ~ 2μg/kg on recovery levels of 60% to 120%.
9.3 Precision
≤30% relative standard deviation in this method and inter - batch relative standard deviation of ≤30%.
Appendix A
Chromatogram
Figure A.1 ammonia standard solution wherein the sulfone of the present ion mass chromatogram (0.5μg/L)
Figure A.2 wherein the sample blank pig liver tissue ion mass chromatogram
Figure A.3 pig liver tissue sample blank add ammonia present sulfones wherein the ion mass chromatogram (0.5μg/kg)
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