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GB 29700-2013: Determination of Clopidol residues in milk by Gas Chromatography-mass Spectrometric method
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Determination of Clopidol residues in milk by Gas Chromatography-mass Spectrometric method
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GB 29700-2013
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Basic data
| Standard ID | GB 29700-2013 (GB29700-2013) |
| Description (Translated English) | Determination of Clopidol residues in milk by Gas Chromatography-mass Spectrometric method |
| Sector / Industry | National Standard |
| Classification of Chinese Standard | C53 |
| Classification of International Standard | 67.020 |
| Word Count Estimation | 10,179 |
| 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 clopidol residue detection sample preparation, gas chromatography mass spectrometry determination. This standard applies to milk clopidol residue testing. |
GB 29700-2013: Determination of Clopidol residues in milk by Gas Chromatography-mass Spectrometric method
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Determination of Clopidol residues in milk by Gas Chromatography-mass Spectrometric method
National Standards of People's Republic of China
National Food Safety Standard
Determination of milk 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 milk residues clopidol
Gas chromatography - mass spectrometry
1 Scope
This standard specifies the milk clopidol Residues sample preparation and gas chromatography - mass spectrometry method.
This standard applies to chloropyridine hydroxyalkyl residues detected in milk.
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 smart clopidol controlled amount 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 6
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
An appropriate amount of fresh or frozen or blank test milk and mix well.
--- 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 concentrations of 5,10,20,100,250 and 500μg/L of matrix-matched series of standard solution, the air supply
Chromatography - mass spectrometry. To measure peak area for the vertical axis, corresponding to the concentration of standard solution as abscissa, the standard curve. Seeking return
Equations and correlation coefficient.
7.2 extract
Sample Weigh 2g ± 0.02g, in 50mL polypropylene centrifuge tube, was added 5mL acetonitrile oscillation 30min. At 4 ℃ 6000r/min
Centrifugal 10min, the supernatant, the residue was added acetonitrile 5mL, extraction was repeated once. The combined supernatant twice, adding isopropanol 2mL, at 50 deg.] C
Rotary evaporated to near dryness, dissolve the residue 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, in
50 ℃ blown dry with nitrogen.
Derived 7.4
The residue was dissolved with 100 L of toluene, was added 100 L derivatizing agents, seal, 80 ℃ derivatization 1h. Cooling, toluene was added 800 L, 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 × 0.25μm), or equivalent person.
7.5.1.2 flow. 0.7mL/min.
7.5.1.3 temperature program. maintained 90 ℃ 1min, at a rate of 30 ℃/min heating to 200 ℃, then to 5 ℃/min was heated to 205 ℃,
Holding 1min, then warmed at 30 ℃/min to 280 ℃, maintained 1min.
7.5.1.4 Interface Temperature. 280 ℃.
7.5.1.5 Inlet temperature. 210 ℃.
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 and 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 milk and milk clopidol blank extract ions
Chromatogram 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.
--- for X-try clopidol the feed content, in micrograms per kilogram (μg/kg);
A --- sample solution clopidol peak area;
cS --- matrix blank standard working solution concentration of clopidol, in micrograms per liter (μg/L);
V --- final sample volume in milliliters (mL);
--- the AS standard working solution matrix blank clopidol peak area;
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 2μg/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 110%.
9.3 Precision
The relative standard deviation of the method ≤20%, inter-assay relative standard deviation ≤20%.
Appendix A
Chromatogram
a)
b)
c)
d)
e)
Figure A.1 clopidol ion chromatogram of the standard solution (20ng/mL)
a)
b)
c)
d)
e)
Figure A.2 milk sample blank ion chromatogram
a)
b)
c)
d)
e)
Figure A.3 milk sample blank add clopidol ion chromatogram (10μg/kg)
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