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GB 23200.78-2016: Food safety national standard -- Meat and meat products -- Determination of the content of carbamate residues -- Gas chromatographic method
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Food safety national standard -- Meat and meat products -- Determination of the content of carbamate residues -- Gas chromatographic method
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GB 23200.78-2016
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Basic data | Standard ID | GB 23200.78-2016 (GB23200.78-2016) | | Description (Translated English) | Food safety national standard -- Meat and meat products -- Determination of the content of carbamate residues -- Gas chromatographic method | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 10,125 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 0641-2011 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of 2016 | | Issuing agency(ies) | National Health and Family Planning Commission of the People's Republic of China, State Food and Drug Administration | GB 23200.78-2016: Food safety national standard -- Meat and meat products -- Determination of the content of carbamate residues -- Gas chromatographic method
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Food safety national standard - Meat and meat products - Determination of the content of carbamate residues - Gas chromatographic method
National Standards of People's Republic of China
GB
Instead of SN/T 0641-2011
National standards for food safety
Determination of the content of carbamate in meat and meat products
Gas chromatography
National food safety standards-
Determination of crotoxyphos residues in meats and meat products
Gas chromatography
2016-12-18 Release.2017-06-18 Implementation
National Health and Family Planning Commission of the People 's Republic of China
Issued by the Ministry of Agriculture of the People 's Republic of China
State Administration of Food and Drug Administration
Foreword
This standard replaces SN/T 0641-2011 "Method for the determination of the amount of carbazole in the import and export of meat and meat products".
Compared with SN/T 0641-2011, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the name and scope of the "import and export of meat and meat products" to "meat and meat products";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN 0641-1997.
National standards for food safety
Meat and meat products - Determination of the content of carbamate residues - Gas chromatographic method
1 Scope
This standard specifies the determination of the amount of carbamate residues in meat and meat products
This standard applies to pork, sausage and lunch meat and other meat and meat products in the determination of the residual amount of carbamylate, other food can refer to the implementation.
2 normative reference documents
The following documents are indispensable for the application of this document. For dated references, only the dated edition applies to this article
Pieces. For undated references, the latest edition (including all modifications) applies to this document.
GB 2763 National Standard for Food Safety - Maximum Residue Limit of Pesticides in Foodstuffs
GB/T 6682 Analytical laboratory water specifications and test methods
3 principle
The residual carbamate in the sample was extracted with a mixture of cyclohexane-ethyl acetate and the extract was purified by gel permeation chromatography.
Photometric detector gas chromatograph determination, external standard method quantitative. If necessary, can be confirmed by gas chromatography-mass spectrometry.
4 reagents and materials
Unless otherwise specified, all reagents are of analytical grade and water is in accordance with the primary water specified in GB/T 6682.
4.1 Reagents
4.1.1 Acetone (C7H6O). Chromatographic purity.
4.1.2 Cyclohexane (C6H12). Chromatographic Purification.
4.1.3 Ethyl acetate (C4H8O2). Chromatographic purity.
4.2 solution preparation
4.2.1 cyclohexane-ethyl acetate (1 1, volume ratio). take 100 mL of cyclohexane, add 100 mL of ethyl acetate, shake back. The
4.2.2 anhydrous sodium sulfate. 650 ℃ burning 4 h, stored in a sealed container in reserve.
4.3 standards
4.3.1 Bareto phosphorus standard (Crotoxyphos, C14H19O6P, CAS. 7700-17-6). purity ≥ 99%.
4.4 standard solution preparation
4.4.1 Batch phosphorus standard solution. accurately weighed the appropriate amount of standard phosphorus poisonants, with acetone prepared into a concentration of about 1.0 mg/mL standard reserve
Liquid, and then need to use acetone diluted to the appropriate concentration of standard working solution. Standard stock solution in 0 ~ 4 ℃ refrigerator to save, valid for 12
Month, the standard working fluid in the 0 ~ 4 ℃ refrigerator to save, valid for 6 months.
5 instruments and equipment
5.1 Gas Chromatograph. Flame photometric detector with phosphor filter (526nm).
5.2 gel permeation chromatography. equipped with unit pump, fraction collector.
5.3 Centrifuge. speed greater than 3000 r/min.
5.4 Electronic balance. accurate to 0.0001 g.
5.5 homogenizer.
5.6 Rotary evaporator.
5.7 Concentrated bottles. 100 mL.
5.8 Organic phase microporous membrane. 0.45 m.
5.9 anhydrous sodium sulfate column. column length 7 cm, diameter 2 cm barrel funnel containing about 3 cm anhydrous sodium sulfate.
6 Preparation and storage of samples
6.1 Preparation of the sample
Will take all the samples, shrink out with a representative sample of not less than 500g, the sampling site according to GB 2763 Appendix A, the mashed
Machine fully mashed evenly, are divided into two, respectively, into a clean container, sealed, marked mark.
6.2 Sample storage
The sample was stored at -18 ° C or lower. During the operation of the sample preparation, the sample should be prevented from being contaminated or the content of the residue can be changed
The
7 Analysis steps
7.1 Extraction
Weigh the sample about 10.0 g (accurate to 0.1 g) in a 50 mL centrifuge tube, add 10 g of anhydrous sodium sulfate, stir with a glass rod
And mixed with the sample, then add 20 mL of cyclohexane-ethyl acetate (1 1, volume ratio), homogeneous 2min, 3000r/min centrifugation 3 min,
The upper organic phase was passed through an anhydrous sodium sulfate column and collected in a 100 mL concentration flask. The residue was washed with 40 mL of cyclohexane-ethyl acetate (11,
Volume ratio) The extracts were extracted twice in the same manner as described above, concentrated to about 5 mL at 40 ° C, and the extract was transferred to a 10 mL scale test
And the mixture was washed three times with 3 mL of cyclohexane-ethyl acetate (1 1, by volume), and the washing solution was combined in a graduated tube.
Cyclohexane-ethyl acetate (1 1, volume ratio) to 10 mL, over 0.45 m filter, to be gel permeation chromatography (GPC) purification.
7.2 Purification
7.2.1 Gel permeation chromatography (GPC) purification
7.2.2 Gel Permeation Chromatographic Conditions
A) Gel purification column. column length 400 mm, inner diameter 25 mm, Bio Beads S-X3, or equivalent;
B) mobile phase. cyclohexane-ethyl acetate (1 1, volume ratio);
C) Flow rate. 5.0 mL/min;
D) sample dosing loop. 5.0 mL;
E) Pre-leaching time. 17 min;
F) Gel permeation chromatograph equilibration time. 5 min;
Collection time. 17 ~ 30 min.
7.2.3 Gel Permeation Chromatography Purification steps
10 mL of the purified liquid was purged according to the conditions specified in 7.2.2, and the collected components were concentrated at room temperature and the mixture was concentrated.
1.0mL acetone dissolved in volume, gas chromatographic determination.
7.3 Determination
7.3.1 Gas Chromatographic Reference Conditions
A) Column. HP-5, column length 30 m, inner diameter 250 μm, film thickness 0.25 μm, or equivalent;
B) Carrier gas. nitrogen, purity ≥99.99%, 1.5mL/min;
C) tail gas. nitrogen, purity ≥ 99.99%, 60mL/min;
D) hydrogen. 75 mL/min;
E) air. 100 mL/min;
F) column temperature. initial temperature of 180 ℃, keep 1 min, at 10 ℃/min rate increased to 280 ℃, keep 5min;
G) Inlet temperature. 250 ° C;
H) Detector temperature..200 ° C;
I) Injection volume. 1 μL;
J) Injection method. no split injection.
7.3.2 Chromatographic determination
According to the sample of phosphorus poisonous phosphorus content, select the peak area and sample solution similar to the standard working solution. Standard working solution and sample solution of poisonous phosphorus
The response value should be within the linear range of the instrument detection. Standard working fluid and sample solution should be equal to the volume of plug-in injection determination. Under the above chromatographic conditions,
The retention time of the drug is about 6.67 min. The gas chromatogram of the standard substance of the toxic substance is shown in Appendix A and quantified by the external standard method.
7.4 Gas Chromatography - Mass Spectrum Confirmation
7.4.1 Gas Chromatography - Mass Spectrometry Reference Conditions
A) Column. Rtx-5MS, column length 30 m, inner diameter 250 μm, film thickness 0.25 μm, or equivalent;
B) Carrier gas. helium, purity ≥99.99%, 1.5mL/min;
C) Column temperature.
D) the program temperature. the initial temperature of 180 ℃, keep 1 min, at 10 ℃/min rate increased to 280 ℃, keep 5 min;
E) Inlet temperature. 250 ° C;
F) chromatographic - mass spectrometer interface temperature. 280 ° C;
G) Injection volume. 1 μL;
H) injection method. no shunt, 1min after the opening valve;
I) ionization energy. 70 eV;
J) ionization mode. EI;
K) Measurement method. ion monitoring mode;
L) monitoring of ions (m/z). 193,166,127,105;
M) solvent delay. 3 min.
7.4.2 Confirmation of mass spectrometry
If the sample solution and the standard solution of the gas chromatogram, in the same retention time there is a peak, you can confirm it by mass spectrometry. Benchmarking
The quasi-solution and sample solution were determined according to the conditions specified in 7.4.1.
7.5 blank experiment
In addition to the sample, according to the above determination steps.
8 results are calculated and expressed
Use the chromatographic data processor or calculate the amount of carbamate in the sample by the following formula (1).
MΑi
VCiAi
.. (1)
Where.
The residual amount of carbamate in the sample, in milligrams per kilogram (mg/kg);
The peak height or peak area of carbamate in sample solution;
Ci - the concentration of carbamate in standard working fluid, in micrograms per milliliter (g/mL);
V - the final volume of the sample volume, in milliliters (mL);
Ais - the standard working fluid in the peak or peak area of baubicin;
M - the mass of the sample represented by the final sample, in grams (g).
Note. The result of the calculation shall be deducted from the blank value. The result of the measurement shall be expressed as the arithmetic mean of the parallel measurement, and two valid digits shall be retained.
9 precision
9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix C requirements.
9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix D requirements.
10% limit and recovery rate
10.1 Quantitation limits
The limit of quantification of this method is 0.01 mg/kg.
10.2 Recovery rate
When the levels were 0.01 mg/kg, 0.05 mg/kg, 0.1 mg/kg, the recovery rates for the addition of carbamate were given in Appendix B.
Appendix A
(Informative)
Standard Gas Chromatography
Figure A.1 Gas Chromatogram of Batch Phosphorus Standard
Appendix B
(Informative)
This method adds concentration and recovery range
Table B.1 This method adds concentration and recovery range
Sample name Add concentration (mg/kg) Recovery rate range (%) Variation coefficient (%)
pork
0.010 73.0 ~ 96.0 9.02
0.050 79.4 ~ 98.8 7.22
0.100 89.5 ~ 101.3 4.11
sausage
0.010 71.0 to 86.0 7.02
0.050 81.0 ~ 94.0 4.89
0.100 84.5 ~ 103.3 7.23
Canned luncheon meat
0.010 71.0 to 101.0 10.47
0.050 74.6 ~ 99.5 9.65
0.100 75.6 ~ 94.6 6.96
Appendix C
(Normative appendix)
Laboratory repeatability requirements
Table C.1 Laboratory repeatability requirements
Measured component content
Mg/kg
Precision
0.001 36
> 0.01
> 1 14
Appendix D
(Normative appendix)
Inter-laboratory reproducibility requirements
Table D.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
Precision
0.001 54
> 0.01
> 1 19
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