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GB 23200.22-2016: Food safety national standard -- Determination of residual residues in nuts and nut products by liquid chromatography
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Food safety national standard -- Determination of residual residues in nuts and nut products by liquid chromatography
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GB 23200.22-2016
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Basic data | Standard ID | GB 23200.22-2016 (GB23200.22-2016) | | Description (Translated English) | Food safety national standard -- Determination of residual residues in nuts and nut products by liquid chromatography | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 10,128 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 0647-2013 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.22-2016: Food safety national standard -- Determination of residual residues in nuts and nut products by liquid chromatography
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Food safety national standard - Determination of residues residual in nuts and nut products by liquid chromatography
National Standards of People's Republic of China
GB
Instead of SN 0647-2013
National standards for food safety
Determination of the Residue in the Nuts and Nuts
Liquid chromatography
National food safety standards-
Determination of maleic hydrazide residue in nuts and nut products
Liquid 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 0647-2013 "Determination of the amount of inhibitory residues in nuts and nuts in nuts and nuts". High performance liquid chromatography.
Compared with SN/T 0647-2013, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- "Import and export nuts and nuts" in the standard name to "nuts and nuts".
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 0647-2013
-SN 0647-1997.
National standards for food safety
Determination of residual residues in nuts and nut products by liquid chromatography
1 Scope
This standard specifies the preparation of nutrient and nutrient detection in nuts and nuts.
This standard applies to walnut and products, chestnut and products in the determination of the remaining amount of buds, 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 samples were degreased with n-hexane, extracted with methanol, purified by C18 column, and analyzed by high performance liquid chromatography with UV detector.
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 Methanol (CH3OH). Chromatographic Purification.
4.1.2 n-hexane (C6H14). pure chromatography.
4.1.3 Ammonium acetate (CH3COONH4).
4.1.4 Sodium hydroxide (NaOH).
4.2 solution preparation
4.2.1 Ammonium acetate solution (0.02 mol/L). Weigh 1.54 g of ammonium acetate, add water to a volume of 1000 mL.
4.2.2 sodium hydroxide solution (0.01 mol/L). Weigh 0.40 g sodium hydroxide, add water to volume to 1000 mL, shake back.
4.3 standards
4.3.1 Constituent granules. Maleic hydrazide, C4H4N2O2, CAS number. 123-33-1, purity ≥99.9%.
4.4 standard solution preparation
4.4.1 suppression of buds standard reserve solution. accurately weighed amount of anti-budding standard material, with sodium hydroxide solution prepared into 1 mg/mL standard
Stock solution, the standard solution away from 0 ℃ ~ 4 ℃ preservation, shelf life of 6 months.
4.4.2 suppression of buds standard working solution. According to the testing requirements, respectively, to absorb the standard reserve solution in the volumetric flask, with sodium hydroxide dissolved
Liquid dilution to the standard preparation of the appropriate concentration of the standard working solution, the standard working solution away from 0 ℃ ~ 4 ℃ preservation, shelf life of 1
Month.
4.5 Materials
4.5.1 C18 solid phase extraction column. 3 mL 500 mg, or equivalent. Followed by 4 mL of methanol and 4 mL of sodium hydroxide solution activated after use.
5 instruments and equipment
5.1 High Performance Liquid Chromatograph with UV or Diode Array Detector.
5.2 Electronic balance. 0.01 g and 0.0001 g.
5.3 Rotary Evaporator.
5.4 homogenizer. speed of not less than 10000 r/min.
5.5 Centrifuge. speed not less than 6000 r/min.
5.6 Scroll Mixer.
5.7 sample grinder.
5.8 Sieve. 2.0 mm round hole sieve.
5.9 template.
6 Preparation and storage of samples
6.1 Preparation of the sample
The edible part of the original sample is reduced to about 500 g, and the sampling site is carried out according to GB 2763 Appendix A and crushed with a sample shredder
Through 20 mm round hole sieve particles. Fully mixed, prepared samples are divided into two, into a clean sample container, sealed and marked
mark.
6.2 Sample storage
Keep the sample below 5 ° C in dark.
During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue.
7 Analysis steps
7.1 to fat
Weigh 2.5 g sample (accurate to 0.01 g) in 50 mL centrifuge tube, add 5 mL of water, vortex and mix for 30 min, add 20 mL
Hexane homogeneous 1 min, 6000 r/min centrifugal 5 min, discarded n-hexane layer; add 20 mL n-hexane according to the above steps re-degreasing once, discarded
N-hexane layer.
7.2 Extraction
Add 20 mL of methanol to the centrifuge tube, homogenize 1 min, 6000 rpm/min centrifugation 5 min, the methanol layer carefully removed to filter 100 mL
The residue was extracted twice with 20 mL of methanol and the combined extracts were vortexed at about 40 ° C to about 8 mL in the same heart,
With nitrogen to about 2 mL, add 3 mL of sodium hydroxide solution to be purified.
7.3 purification
The above mixed solution was passed through a C18 column, eluted with 4 mL of sodium hydroxide solution and set to 10 mL for high performance liquid chromatography
Determination.
7.4 determination
7.4.1 High Performance Liquid Chromatography Reference Conditions
A) Wavelength. 330 nm.
B) Column. silica gel column, 3.5 μm, 4.6 mm × 150 mm, or equivalent.
C) Column temperature. 40 ° C.
D) Mobile phase. ammonium acetate solution (4.2.1).
E) Mobile phase flow rate. 0.60 mL/min.
F) Injection volume. 20 μL.
7.4.2 Chromatographic determination
According to the content of buds in the sample solution, the standard working solution with similar peak area is selected, and the standard working solution and sample solution
The response values of the standard working solution and the sample solution should be within the linear range of the instrument detection. In the above chromatogram
Under the conditions, the retention time is about 3.10 min.
See Figure A in Appendix A for standard chromatograms.
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 according to formula (1) to calculate the content of curd in the sample.
Ai × Csi × V
ASi × m (1)
Where.
X - Residue content in the sample in milligrams per kilogram (mg/kg);
The peak area of the buds in the sample solution;
The peak area of the standard working solution of ASi -
V - the final volume of the sample solution in milliliters (mL);
Csi - Concentration of standard working solution in micrograms per milliliter (μg/mL);
M - the amount of sample represented by the final sample solution in grams (g).
X =
Note. The result of the calculation should be deducted from the blank value. The result of the measurement is expressed by the arithmetic mean of the parallel measurement, and the two valid digits are 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 0.2 mg/kg.
10.2 Recovery rate
When adding levels of 0.2 mg/kg, 0.4 mg/kg, 2 mg/kg, the addition rates for the addition of buds in different matrices are given in Appendix B.
Appendix A
(Informative)
Suppose the standard of the standard
Figure A map of the standard (1.5 mg/L)
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 Name Add Concentration (mg/kg) Recovery (%)
walnut
0.2 82.5 ~ 95.5
0.4 81.2 to 94.8
2.0 90.2 to 100.2
Honey walnut
0.2 83.5 to 96.5
0.4 80.2 to 101.2
2.0 91.0 to 104.9
Chestnut
0.2 80.5 to 94.0
0.4 83.4 to 97.8
2.0 90.2 to 100.6
Sugar fried chestnut
0.2 81.5 to 99.5
0.4 84.2 to 97.8
2.0 90.2 to 102.6
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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