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GB 29699-2013: Determination of Clopidol residues in chicken muscle by Gas Chromatography-mass Spectrometric method
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Determination of Clopidol residues in chicken muscle by Gas Chromatography-mass Spectrometric method
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GB 29699-2013
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Basic data
| Standard ID | GB 29699-2013 (GB29699-2013) |
| Description (Translated English) | Determination of Clopidol residues in chicken muscle by Gas Chromatography-mass Spectrometric method |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | C53 |
| Classification of International Standard | 67.020 |
| Word Count Estimation | 10,151 |
| 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 chicken muscle tissue clopidol residue detection sample preparation, gas chromatography mass spectrometry. This standard applies to chicken muscle tissue clopidol residues measured. |
GB 29699-2013: Determination of Clopidol residues in chicken muscle by Gas Chromatography-mass Spectrometric method
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Determination of Clopidol residues in chicken muscle by Gas Chromatography-mass Spectrometric method
National Standards of People's Republic of China
National Food Safety Standard
Determination of chicken muscle tissue pyridine residues clopidol
Gas chromatography - 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 chicken muscle tissue pyridine residues clopidol
Gas chromatography - mass spectrometry
1 Scope
This standard specifies the sample preparation and gas chromatography chicken muscle tissue clopidol of Residues - mass spectrometry.
This standard is applicable to the determination of chicken muscle tissue pyridine chlorine hydroxyalkyl 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 clopidol, extracted with acetonitrile, basic alumina column purification, N, O- bis (trimethylsilyl) trifluoroacetamide and three
Chlorosilane derivatization gas chromatography - mass spectrometry, external standard.
4 Reagents and Materials
The following reagents used, unless otherwise stated are analytical reagents, water as a water line with GB/T 6682 provisions.
Clopidol Reference Sample 4.1. content of ≥99%.
Anhydrous sodium sulfate 4.2. Before use in the muffle furnace at 500 ℃ 5h, cooled, through a 100 mesh sieve, spare.
4.3 basic alumina. muffle furnace before use after 300 ℃ calcined 3h, cooled water was added 100g per 5mL, mixing, desiccator over
Night and set aside.
4.4 N, O- bis trimethylsilyl trifluoroacetamide.
4.5 trimethylchlorosilane.
4.6 acetonitrile.
4.7 toluene. chromatography.
4.8 Helium. purity ≥99.999%.
4.9 derivatizing agents. taking N, O- bis trimethylsilyl trifluoroacetamide 99mL, add trimethylsilyl chloride 1mL, mix.
4.10 Alumina column. alumina column chromatography using a plug of glass with a 30mm × 15mm, with the sand core plate G3, charged with an appropriate amount of B to
Nitriles, then loaded over anhydrous sodium 1cm high, intermediate high mounted 4cm basic alumina, and then loaded to the top 1cm high sulfate, and gently knock
Uniform solid fill, the standby.
4.11 100μg/mL clopidol standard stock solution. Weigh accurately clopidol reference substance 10mg, in 100mL flask with methanol solution
Solution and dilute to volume, formulated at a concentration of 100μg/mL of stock standard solution clopidol. -20 ℃ below, valid for six months.
4.12 1μg/mL clopidol standard working solution. precise amount of 100μg/mL standard stock solution clopidol 1.0mL, in 100mL
Volumetric flask, dilute to the mark with methanol, formulated at a concentration of 1μg/mL of the working standard solution clopidol stored 2 ℃ ~ 8 ℃, valid
1 week.
5 instruments and equipment
5.1 Gas chromatography - mass spectrometry. with electron impact ionization (EI).
5.2 Analytical balance. a sense of volume 0.00001g.
5.3 Balance. a sense of the amount of 0.01g.
5.4 high-speed refrigerated centrifuge.
5.5 rotary evaporator.
5.6 shaker.
5.7 polypropylene centrifuge tube. 50mL.
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
Or less at -20 ℃.
Determination Step 7
7.1 Preparation of matrix-matched standard curve
The precise amount of 1μg/mL clopidol appropriate amount of working standard solution, were added to the extracted, the purification step of the processing parts of the blank sample 6
Eluate by derivatization, to obtain the concentration of 5,10,20,100,250 and 500μg/L of matrix-matched series of standard solution, gas phase color
Spectroscopy - mass spectrometry. To measure peak area for the vertical axis, corresponding to the concentration of standard solution as abscissa, the standard curve. Seeking regression equation
And the correlation coefficient.
7.2 extract
Sample Weigh 5g ± 0.05g, in 50mL polypropylene centrifuge tube, acetonitrile was added 10mL, homogeneous 1min, oscillation 20min. 4 ℃,
6000r/min centrifugal 10min, the supernatant, the residue was extracted with acetonitrile is repeated once 10mL. The combined supernatant twice, adding isopropanol
5mL, 50 deg.] C at a rotary evaporator to near dryness. The residue was dissolved with acetonitrile standby 5mL.
7.3 Purification
Basic alumina column activated with 15mL acetonitrile, taking stock solution through the column, the natural flow of dry acetonitrile was added 10mL, collecting eluate,
50 deg.] C and blown dry with nitrogen.
Derived 7.4
The residue was dissolved in toluene was added 100 L, 100 L adding derivatizing agent, seal, 80 ℃ derivatization 1h. Cooling, toluene was added 800 L, for
Gas Chromatography - Mass Spectrometry.
7.5 Determination
7.5.1 Gas chromatographic conditions
7.5.1.1 Column. phenylmethyl silicone capillary column (30m × 0.25mm, film thickness 0.25μm), or equivalent person.
7.5.1.2 flow. 0.8mL/min.
7.5.1.3 temperature program. 100 ℃ 1min, to a rate of 30 ℃/min heating to 200 ℃, then to 5 ℃/min was heated to 205 ℃, Paul
Temperature 1min, then 30 ℃/min was heated to 280 ℃, maintained 1min.
7.5.1.4 Interface Temperature. 280 ℃.
7.5.1.5 Inlet temperature. 220 ℃.
7.5.1.6 Injection mode. splitless.
7.5.1.7 Injection volume. 1μL.
7.5.2 MS conditions
7.5.2.1 ionization mode. electron ionization (EI).
7.5.2.2 Ion source temperature. 230 ℃.
7.5.2.3 Scan mode. Selected ion monitoring, qualitative ion m/z212,214,248 and 263, qualifier ion m/z248.
7.5.3 Assay
7.5.3.1 qualitative determination
Samples with the standard peak retention time is not more than 2s.
Detecting at least four characteristic ions, i.e. 212,214,248,263, wherein.
248 base peak ion is selected;
SIM relative intensity of 214,263 (base peak ratio) of not more than 30% relative intensity corresponding to a standard average of selected ion;
SIM 212 relative intensity ratios (base peak) does not exceed the corresponding selection criteria relative ion intensity of 25% of the average.
Clopidol trimethylsilyl ether derivative spectrum and the extracted ion chromatogram, add chicken and chicken clopidol blank tissue extracts
Ion chromatogram given in Appendix A.
Quantitative determination 7.5.3.2
Take the sample solution and the volume of matrix blank sample standard solutions and other injections of measured peak area base peak (m/z248) (peak height) as a single point
Multi-point calibration, external standard. Matrix blank sample solution and the standard solution the response value clopidol linear range of the instrument to be detected
Around inside.
7.6 Blank test
But without addition of the sample, the same steps employed in parallel operation.
Calculation and Expression of Results 8
Residues of the specimens clopidol (μg/kg) according to formula (1).
X =
A × cS × V
AS × m
(1)
Where.
Concentration of the sample of X---- clopidol, in units of micrograms per kilogram (μg/kg);
Sample A --- clopidol peak area;
--- the AS peak area of standard solution of clopidol;
Standard solution concentration cS --- clopidol, in units of micrograms per liter (μg/L);
V --- final sample 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 detection sensitivity, accuracy and precision
9.1 Sensitivity
The detection limit of the method was 1μg/kg, the limit of quantitation of 5μg/kg.
9.2 Accuracy
This method of adding 5μg/kg ~ 100μg/kg on recovery levels of 60% to 120%.
9.3 Precision
The relative standard deviation of the method ≤20%, inter-assay relative standard deviation ≤20%.
Appendix A
Chromatogram
Figure A.1 clopidol ion chromatogram of the standard solution (10ng/mL)
Figure A.2 chicken muscle tissue ion chromatogram of blank sample
Figure A.3 chicken muscle tissue sample blank add clopidol ion chromatogram (10μg/kg)
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