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GB 29690-2013: Determination of marker residues of Nicarbazin in animal derived food by Liquid Chromatography-tandem Mass Spectrometric method
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Determination of marker residues of Nicarbazin in animal derived food by Liquid Chromatography-tandem Mass Spectrometric method
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GB 29690-2013
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Basic data
| Standard ID | GB 29690-2013 (GB29690-2013) |
| Description (Translated English) | Determination of marker residues of Nicarbazin 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 | 12,111 |
| 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 nicarbazin residues markers 4, 4 dinitrobenzene biuret residue detection sample preparation, liquid chromatography tandem mass spectrometry. |
GB 29690-2013: Determination of marker residues of Nicarbazin in animal derived food by Liquid Chromatography-tandem Mass Spectrometric method
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Determination of marker residues of Nicarbazin in animal derived food by Liquid Chromatography-tandem Mass Spectrometric method
National Standards of People's Republic of China
National Food Safety Standard
Animal foods nicarbazin residues markers
Determination of residual 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
Animal foods nicarbazin residues markers
Determination of residual liquid chromatography - tandem mass spectrometry
1 Scope
This standard specifies the animal food residue nicarbazin marker 4,4-dinitrophenyl biuret Residues sample preparation and liquid chromatography
Spectrum - tandem mass spectrometry.
This standard applies to chicken eggs and muscle tissue markers nicarbazin residues were detected 4,4'-dinitro diphenyl urea 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
The sample of residual 4,4-dinitrobenzene biuret, extracted with acetonitrile, hexane degreasing, extracted with 75% aqueous methanol solution, liquid chromatography - tandem
Mass spectrometry, as internal standard.
4 Reagents and materials
The following reagents used, unless otherwise stated who were of analytical reagent; water as a water line with GB/T 6682 provisions.
4.1 4,4-dinitro-stilbene urea reference. content of ≥98.0%.
4.2 4,4-dinitro-stilbene urea -D8 reference. content of ≥98.0%.
4.3 Acetonitrile. chromatographically pure.
4.4 Methanol. HPLC grade.
4.5 over anhydrous sodium sulfate.
4.6 n-hexane.
4.7 ammonium acetate.
4.8 dimethylformamide.
4.9 0.1mol/L ammonium acetate solution. Take ammonium acetate 1.93g, dissolve and dilute to 250mL with water.
4.10 75% aqueous methanol. Methanol 75mL, dissolved and diluted to 100mL with water.
4.11 75% saturated aqueous methanol n-hexane. Take 75% aqueous methanol 100mL, 100mL of n-hexane was added, shake and let stand stratification,
The upper liquid.
4.12 1mg/mL4,4'- dinitro diphenyl ureas are standard stock solution. Weigh accurately 4,4'-dinitro-stilbene urea reference substance 10mg, in
10mL volumetric flask, dissolved with dimethyl formamide and diluted to the mark, formulated at a concentration of 4,4-dinitro 1mg/mL standard were diphenylurea
Quasi stock solution. 2 ℃ ~ 8 ℃ storage period of three months.
4.13 10μg/mL4,4'- urea-dinitro-stilbene standard working solution. precise amount of 1mg/mL4,4'- dinitro diphenyl ureas are standard stock
1.0 mL solution, in 100mL flask, dissolved in methanol and diluted to the mark, formulated at a concentration of 4,4-dinitro-10μg/mL were two
Phenylurea standard working solution. -18 ℃, valid for three months.
4.14 1mg/mL4,4'- dinitro diphenyl urea -D8 are standard stock solution. Weigh accurately 4,4'-dinitro-stilbene urea reference -D8
10mg, in 10mL volumetric flask, dissolve and dilute to volume with dimethylformamide, prepared at a concentration of 4,4-dinitro 1mg/mL of
Diphenylurea -D8 are standard stock solution. 2 ℃ ~ 8 ℃ storage period of three months.
4.15 10μg/mL4,4'- dinitro-stilbene urea -D8 standard working solution. precise amount of 1mg/mL4,4'- dinitro-stilbene urea -D8
1.0 mL standard stock solution, to a 100mL flask, dissolved in methanol and diluted to the mark, formulated at a concentration of 10μg/mL 4,4'-bis
Nitro stilbene urea -D8 working standard solution. -18 ℃, valid for three months.
5. Apparatus
5.1 liquid chromatography - tandem mass spectrometry. ion source distribution.
5.2 Analytical balance. a sense of volume 0.00001g.
5.3 Balance. a sense of the amount of 0.01g.
5.4 a vortex.
5.5 centrifuge.
5.6 Nitrogen blowing instrument.
5.7 centrifuge tube. 50mL.
5.8 Membrane. 0.2μm.
Preparation and Storage of sample 6
6.1 Preparation of the sample
6.1.1 eggs
An appropriate amount of fresh or frozen egg white or test, peeled, 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.
6.1.2 chicken muscle
Fresh or frozen 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
Or less at -20 ℃.
Determination Step 7
7.1 Extraction and purification
Sample Weigh 2g ± 0.02g, in 50mL centrifuge tubes, was added 10μg/mL4,4'- dinitro-stilbene working standard solution of urea suitable -D8
Amount of anhydrous sodium sulfate 2g, 8 mL of acetonitrile, vortexed 0.5min, ultrasonic 5min, 5000r/min centrifugal 10min, supernatant at
40 ℃ dry nitrogen, was added 75% aqueous methanol saturated with hexane 1mL, scroll 10s, plus 1.0 mL of 75% aqueous methanol, sufficient
Vortexed, allowed to stand in a water bath at 40 ℃ 5min, 2000r/min centrifugal 5min, the supernatant and the lower layer, membrane filtration, for liquid chromatography - tandem
Mass Spectrometry.
7.2 Preparation of standard curve
The precise amount of 10μg/mL4,4'- dinitro-stilbene working standard solutions of urea and 10μg/mL4,4'- dinitro-stilbene standard urea -D8
Working fluid amount, diluted with 75% aqueous methanol solution, were formulated as 4,4'-dinitro diphenyl urea concentration -D8 are 100ng/mL and 4,4'-
Dinitro-stilbene 2,10,20,50,200 and urea concentration is 500ng/mL series control solution for liquid chromatography - tandem mass spectrometry.
A characteristic ion mass chromatogram peak area for the vertical axis, the standard solution at abscissa, the standard curve. Seeking regression equation and correlation
coefficient.
7.3 Determination
7.3.1 LC Conditions
7.3.1.1 Column. C18 (150mm × 2.1mm, particle size 5μm), or equivalent person.
7.3.1.2 Mobile phase. methanol 0.1mol/L ammonium acetate solution (75 25, volume ratio).
7.3.1.3 flow rate. 0.2mL/min.
7.3.1.4 Column temperature. 30 ℃.
7.3.1.5 Injection volume. 20μL.
7.3.2 MS conditions
7.3.2.1 ion source. electrospray ionization source.
7.3.2.2 Scan mode. negative ion scan.
7.3.2.3 Detection mode. multiple reaction monitoring.
7.3.2.4 ionization voltage. 3.0kV.
7.3.2.5 source temperature. 110 ℃.
7.3.2.6 atomizing temperature. 350 ℃.
7.3.2.7 Cone gas flow rate. 50L/h.
7.3.2.8 atomizing gas flow rate. 450L/h.
7.3.2.9 qualitative and quantitative Cone voltage of ion collision energy and are shown in Table 1.
Table 1 DNC and the internal standard qualitative and quantitative Cone voltage of ion collision energy
drug
Qualitative ion pair
m/z
Quantitative ion pair
m/z
Cone voltage
Collision energy
eV
DNC
300.9 > 136.9
300.9 > 106.9
300.9 > 136.9 20
DNC-D8 309.0 > 141.0 309.0 > 141.0 20 18
7.3.3 Assay
Take a sample solution and control solution, as a single or multi-point calibration, according to the internal standard method, the peak area ratio calculation. Sample solution and control solution
4,4'-dinitro-4,4'-stilbene urea and urea-nitro-stilbene -D8 peak area ratio should be within the linear range of the detection instrument. Sample solution
Compared the relative abundance of ions in solution and the standard solution was added blank relative abundance of ions, in accordance with Table 2. And blank control solution
The features added ion mass chromatogram of the sample solution is given in Appendix A.
Table 2 sample solution ion relative abundance tolerance range%
Tolerance relative abundance
> 50 ± 20
20 ~ 50 ± 25
10 ~ 20 ± 30
≤10 ± 50
7.4 Blank test
But without addition of the sample, the same steps employed in parallel operation.
8 and the result of the calculation expression
Single-point calibration.
c =
AA'iScSciS
AiSASc'iS
(1)
Calibration or standard curve by.
AS
A'iS =
cS
c'iS
to obtain a and b b, then
c =
ciS
(A
AiS-
b) (2)
DNC remaining amount in a sample according to formula (3) is calculated.
X =
CV
(3)
Where.
C --- sample solution of 4,4'-dinitro-stilbene urea concentration, in units of nanograms per milliliter (ng/mL);
A --- sample solution of 4,4'-dinitro diphenyl urea of average peak area;
A'iS --- control solution of 4,4'-dinitro-stilbene urea -D8 peak area;
cS --- control solution of 4,4'-dinitro-stilbene urea concentration, in units of nanograms per milliliter (ng/mL);
--- CIS averaged concentration in the sample solution of 4,4'-dinitro diphenyl urea -D8, expressed in nanograms per milliliter (ng/mL);
--- AiS sample solution of 4,4'-dinitro-stilbene urea -D8 peak area;
--- the AS control solution of 4,4'-dinitro-stilbene urea peak area;
c'iS --- control solution of 4,4'-dinitro diphenyl urea -D8 average concentration, expressed in nanograms per milliliter (ng/mL);
--- try feed for X-4,4'-nitro-diphenyl urea residues are, in micrograms per kilogram (μg/kg);
V --- volume of the residue was dissolved in 75% aqueous methanol, 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 detection sensitivity, accuracy and precision
9.1 Sensitivity
The detection limit of the method was 0.5μg/kg, the limit of quantitation was 1μg/kg.
9.2 Accuracy
The method of the present egg sample is added in a concentration of 1μg/kg ~ 10μg/kg, chicken muscle sample concentration of water added in 1μg/kg ~ 300μg/kg
On recovery levels of 80% to 120%.
9.3 Precision
The relative standard deviation of the method ≤20%, inter-assay relative standard deviation ≤20%.
Appendix A
Chromatogram
a)
b)
c)
Description.
1 --- DNC wherein ion mass chromatogram (300.9 > 106.9);
2 --- DNC wherein ion mass chromatogram (300.9 > 136.9);
3 --- DNC-D8 wherein ion mass chromatogram (309.0 > 141.0);
4 --- Blank Organization ion chromatogram (TIC).
FIG A.1 4,4'- dinitro-stilbene urea standard solution and internal standard ion mass chromatogram characterized (4ng/mL)
a)
Figure A.2 chicken muscle tissue sample blank wherein the ion mass chromatogram
b)
c)
Description.
1 --- DNC wherein ion mass chromatogram (300.9 > 106.9);
2 --- DNC wherein ion mass chromatogram (300.9 > 136.9);
3 --- DNC-D8 wherein ion mass chromatogram (309.0 > 141.0);
4 --- Blank Organization ion chromatogram (TIC).
Figure A.2 (continued)
a)
b)
c)
Figure A.3 blank Chicken muscle-dinitro-4,4'-stilbene ureido wherein the sample and the internal standard ion mass chromatogram (2ng/g)
d)
Description.
1 --- DNC wherein ion mass chromatogram (300.9 > 106.9);
2 --- DNC wherein ion mass chromatogram (300.9 > 136.9);
3 --- DNC-D8 wherein ion mass chromatogram (309.0 > 141.0);
4 --- Blank Organization ion chromatogram (TIC).
Figure A.3 (CONTINUED)
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