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GB 23200.105-2016: Food safety national standard -- Meat and meat products -- Determination of carbazate residues -- Liquid chromatography -- Post-column derivatization fluorescence detection
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Food safety national standard -- Meat and meat products -- Determination of carbazate residues -- Liquid chromatography -- Post-column derivatization fluorescence detection
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GB 23200.105-2016
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Basic data | Standard ID | GB 23200.105-2016 (GB23200.105-2016) | | Description (Translated English) | Food safety national standard -- Meat and meat products -- Determination of carbazate residues -- Liquid chromatography -- Post-column derivatization fluorescence detection | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 11,161 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 0122-2011 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.105-2016: Food safety national standard -- Meat and meat products -- Determination of carbazate residues -- Liquid chromatography -- Post-column derivatization fluorescence detection
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Food safety national standard - Meat and meat products - Determination of carbazate residues - Liquid chromatography - post - column derivatization fluorescence detection
National Standard of the People 's Republic of China
GB
0521-200
National standards for food safety
Determination of Carnosilvine Residue in Meat and Meat Products
Liquid Chromatography - Post - column Derivative Fluorescence Detection
National food safety standards-
Determination of carbaryl residue in meat and meat products
HPLC-fluoresce detector with post column derivation
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
Instead of SN/T 0122-2011
Foreword
This standard replaces SN/T 0122-2011 "Determination of Carbendazim Residue in Import and Export Meat and Meat Products Liquid Chromatography - Post-column Derived Fluorescence
Light detection method ".
Compared with SN/T 0122-2011, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the name 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 0122-1992;
-SN/T 0122-2011.
National standards for food safety
Determination of Carnosilvine Residue in Meat and Meat Products
Liquid Chromatography - Post - column Derivative Fluorescence Detection
1 Scope
This standard specifies the liquid and liquid chromatography-post-column derivatization fluorescence detection method for the removal of carbaryl residues in meat and meat products.
This standard applies to the import and export of beef, chicken, shrimp, fish and ham in the determination of the residual amount of decamethrin, other food can refer to
carried out.
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 2763-2014 National Standard for Food Safety - Maximum Residue Limits for Pesticides in Foodstuffs
Analysis of laboratory water specifications and test methods GB/T 6682-2008
3 principle
The residue of the decamethrin in the sample was extracted with a mixture of acetone and petroleum ether. After purification by gel column, the mixture was concentrated and analyzed by high performance liquid chromatography
Separation, after column derivatization, with the fluorescence detector detection, external standard quantitative.
4 reagents and materials
Unless otherwise specified, all reagents are analytical reagent and water is a Class I water specified in GB/T 6682.
4.1 Reagents
4.1.1 Acetonitrile (CH3CN). Chromatographically pure.
4.1.2 Ethyl acetate (C4H8O2). Chromatographic purity.
4.1.3 Cyclohexane (C6H12). Chromatographic Purification.
4.1.4 Acetone (CH3COCH3). Chromatographic pure.
4.1.5 petroleum ether. boiling range 30 ℃ ~ 60 ℃.
4.1.6 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve.
4.1.7 Sodium chloride (NaCl).
4.1.8 post-column derivatization reagents.
4.1.9 o-phthalaldehyde (C8H602, O-Phthaladehyde, OPA).
4.1.10 mercaptoethanol (C2H6OS, Thiofluor).
4.2 solution preparation
4.2.1 NaOH solution (0.2%, m/v). take 2 g NaOH, the volume of water to 1000 mL.
4.2.2 O-phthalaldehyde diluent. borax solution (0.4%, m/v).
4.2.3 O-phthalaldehyde test solution. 945 ml of OPA diluent was injected into the solvent tank and purged with inert gas (nitrogen) for at least 10 min,
100 mg of OPA solids were dissolved in about 10 mL of chromatographic pure methanol and the OPA solution was added to the deoxygenated OPA diluent to dissolve 2 g of mercaptan
Base ethanol solids in 5 mL OPA diluent, added to the tank, covered with cap, open airflow, and then continue to purge for a few minutes,
The valve is gently agitated to make it completely mixed.
4.2.4 Ethyl acetate-cyclohexane mixed solution (1 1, v/v). Take 100 mL of ethyl acetate, add 100 mL of cyclohexane and shake well.
4.3 standards
4.3.1 Carbaryl. Molecular formula C12H11NO2, CAS 63-25-2, purity > 99.5%.
4.4 standard solution preparation
4.4.1 Monazalose standard stock solution. accurately weighed the right amount of methacon standard, dissolved in acetonitrile, 4 ℃ refrigerator, valid for 6
month. Store in 4 ℃ refrigerator.
4.4.2 Carbaryl standard working solution. take a certain amount of standard stock solution, diluted with acetonitrile to the appropriate concentration, 4 ℃ refrigerator, valid for
1 week. Store in 4 ℃ refrigerator.
4.5 Materials
4.5.1 0.45 μm nylon filter.
5 instruments and equipment
5.1 Liquid Chromatography. equipped with fluorescence detectors and post-column derived units.
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 Fully automatic gel chromatograph (with fraction collection concentrator).
5.4 Rotary Evaporator.
5.5 nitrogen blowing instrument.
5.6 Tissue homogenizer.
5.7 Oscillator.
6 Preparation and storage of samples
6.1 Preparation of the sample
6.1.1 meat
All the samples taken, fully mixed and mixed, take a representative sample, the total amount of not less than 500 g, into the cleaning container, sealed
And mark the mark.
6.1.2 canned
The whole sample of the whole pot can be poured out, fully blended mix, take a representative sample, the total amount of not less than 500 g, into the cleaning container
Sealed and marked.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
6.2 Sample storage
Samples should be stored below -18 ° C. In the operation of sampling and sample preparation, the sample should be protected from contamination or changes in content.
The test sample can represent the overall sample.
7 Analysis steps
7.1 Extraction
Weigh the sample 20 g (accurate to 0.01 g), add 100 mL of water in a 100 mL stopper, add water 6 mL (depending on the moisture content of the sample
Water about 20 g, meat is usually about 70%, add water 6 mL), add 40 mL of acetone, homogenate 1 min, add sodium chloride 6 g, shake well,
Plus 30 mL of petroleum ether, shake for 30 min. Take 35 mL of the organic layer supernatant, filtered through anhydrous sodium sulfate in a rotary vial and concentrated to
About 1 mL, add 2 mL of ethyl acetate-cyclohexane solution and re-concentrate, so repeat 3 times. Ethyl acetate - cyclohexane volume of 5 mL, 0.45 μ
M filter filter, to be purified.
7.2 Gel Chromatography (GPC) purification
7.2.1 Gel Chromatographic Purification Reference Conditions
A) Purification column. 400 mm × 30 mm, Bio Beads S-X3, or equivalent.
B) Mobile phase. ethyl acetate-cyclohexane.
C) Flow rate. 5.0 mL/min.
D) Sample loop. 5 mL.
E) Distillate collection section. 10.0 min ~ 15.0 min.
F) purification column balance time. 5 min.
7.2.2 Gel Chromatography Concentration Reference conditions
A) Sample concentration conditions are shown in Table 1.
B) Concentration end point determination. Level sensing mode.
C) Solvent Replacement. 2 mL acetonitrile, repeated twice.
D) constant volume. 1 mL.
7.2.3 Gel Chromatography Purification Procedure
5 mL of the purified liquid according to the conditions specified in 7.2.1 and 7.2.2 purification and concentration, and finally get 1 mL of the solution to be determined.
Table 1 Fraction Concentration Conditions
Concentration Period Concentration Cup Area Temperature (° C) Vacuum (Torr)
Sample concentration process
Zone 1 50 280
Zone 2 52 220
Zone 3 54
Concentration end point arrival process
Zone 1 52 220
Zone 2 53 220
7.3 Determination
7.3.1 Liquid Chromatographic Reference Conditions
A) Column. C18,250 mm x 4.6 mm x 5 μm, or equivalent;
B) Column temperature. 42 ° C;
C) Fluorescence detector. λex 330 nm, λem 465 nm;
D) mobile phase. acetonitrile water (40 60, volume ratio);
E) Flow rate. 1.0 mL/min;
F) Injection volume. 20 L.
7.3.2 post-column derivatization
A) Derivative reagent 1. Hydrolysis reagent, 0.4% sodium hydroxide solution, flow rate 0.4 mL/min;
B) Derivative reagent 2. OPA reagent at a flow rate of 0.4 mL/min;
C) Reactor temperature. hydrolysis temperature is 100 ° C and the temperature is room temperature.
7.3.3 Chromatographic determination
According to the content of kaempferol measured in the sample solution, the standard working fluid with similar concentration should be selected. The response value should be in the linear range
Inside. Under the above liquid chromatographic conditions, the retention time of Carbaryl is 11.1 min, and the chromatogram is shown in Figure A.1 in Appendix A.
7.3.4 Blank test
In addition to the sample, according to the above steps.
8 results are calculated and expressed
According to formula (1) to calculate the content of carnosilane in the sample.
MA
VCA
(1)
Where.
X - The amount of carbaryl in the sample, in milligrams per kilogram (mg/kg);
A - the chromatographic peak area of carbaryl in the sample;
Cs - the concentration of carbaryl in the standard working solution in micrograms per milliliter (μg/mL);
V - the final volume of the sample solution in milliliters (mL);
As - the chromatographic peak area of carbamate in standard working solution;
M - the amount of the final sample, expressed 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, recovery rate
10.1 Quantitation limits
The limit of quantification of this method is 0.005 mg/kg.
10.2 Recovery rate
The recovery rate of norethium is shown in Appendix B.
Appendix A
(Informative)
Monochloride standard chromatogram
Figure A.1 Liquid Chromatography (0.1 μg/mL)
Appendix B
(Informative)
Sample concentration and recovery of the experimental data
Table B.1 Experimental data on the concentration and recovery of the sample
sample
Add level
(Mg/kg)
Recovery rate range
(%)
sample
Add level
(Mg/kg)
Recovery rate range
(%)
Fish
0.005 82.0 ~ 110.0
Ham
0.005 90.0 to 96.0
0.010 89.0 to 107.0 0.010 100.0 to 114.0
0.020 94.0 to 112.5 0.020 97.0 to 115.5
0.050 90.0 to 105.6 0.050 101.6 to 113.6
0.100 92.0 to 111.2 0.100 92.5 to 107.3
beef
0.005 82.0 ~ 98.0
Shrimp
0.005 86.0 ~ 100.0
0.010 86.0 to 99.0 0.010 85.0 to 96.0
0.020 84.5 to 109.5 0.020 87.0 to 105.0
0.050 90.6 ~ 98.0 0.050 88.6 ~ 94.6
0.100 88.4 ~ 98.0 0.100 86.7 ~ 95.1
chicken
0.005 86.0 to 96.0
0.010 89.0 to 97.0
0.020 95.5 to 112.5
0.050 92.0 to 97.2
0.100 85.9 ~ 95.0
5.000 87.7 to 102.5
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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