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GB 23200.32-2016: Food safety national standard -- Determination of butyryl hydrazine residues in foodstuffs by gas chromatography-mass spectrometry
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Food safety national standard -- Determination of butyryl hydrazine residues in foodstuffs by gas chromatography-mass spectrometry
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GB 23200.32-2016
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Basic data | Standard ID | GB 23200.32-2016 (GB23200.32-2016) | | Description (Translated English) | Food safety national standard -- Determination of butyryl hydrazine residues in foodstuffs by gas chromatography-mass spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 10,117 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 1989-2007 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.32-2016: Food safety national standard -- Determination of butyryl hydrazine residues in foodstuffs by gas chromatography-mass spectrometry
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Food safety national standard - Determination of butyryl hydrazine residues in foodstuffs by gas chromatography - mass spectrometry
1.1.1.1.1.2
Instead of SN/T 1989-2007
National standards for food safety
Determination of butyryl hydrazine residues in food
Gas chromatography - mass spectrometry
National food safety standards-
Determination of daminozide residue in foods
Gas chromatography - mass spectrometry
× × × × - × - × release
× × × × × × × × 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
GB
National Standards of People's Republic of China
2016-12-18 Release.2017-06-18 Implementation
Foreword
This standard replaces SN/T 1989-2007 "Determination of Butyryl Hydrazide Residue in Import and Export Food by Gas Chromatography-Mass Spectrometry".
Compared with SN/T 1989-2007, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the name of the "export food" to "food";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 1989-2007.
National standards for food safety
Determination of butyryl hydrazine residues in foodstuffs by gas chromatography - mass spectrometry
1 Scope
This standard specifies the method for the determination of butyryl hydrazide residues in food by gas chromatography-mass spectrometry.
This standard applies to the determination of the residual amount of butyryl hydrazide in peanuts, rice, soybeans, parsley, apples, fish, chicken, tea and honey.
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 unreacted hydrazide residue in the sample was extracted with water, purified by steam distillation, salicylaldehyde derivatization, silica gel solid phase extraction column, and purified by gas chromatography
- mass spectrometer for determination, external standard method quantitative.
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 n-hexane (C6H14). chromatographic purity.
4.1.2 Sodium hydroxide (NaOH).
4.1.3 Sodium chloride (NaCl).
4.1.4 glacial acetic acid (C2H4O2).
4.1.5 Salicylaldehyde (C7H6O2).
4.1.6 Ethyl acetate (C4H8O2). Chromatographic purity.
4.2 solution preparation
4.2.1 Ethyl acetate n-hexane solution (3 97, V/V). Take 30 mL of ethyl acetate, add 970 mL of n-hexane and shake well.
4.2.2 acetic acid solution (10%, v/v). Remove 10 mL of glacial acetic acid by adding 90 mL of water and mix well.
4.2.3 Sodium hydroxide solution (50%, m/v). Weigh 500 g of sodium hydroxide gradually dissolved in 1 L of water, cooled and mixed thoroughly.
4.3 standards
4.3.1 1,1-dimethyl hydrazine, C2H8N2, CAS. 57-14-7). purity ≥98%.
4.4 standard solution preparation
4.4.1 1,1-dimethyl hydrazine reserve solution. accurately weighed the appropriate amount of 1,1-dimethyl hydrazine standard 0.1 g (accurate to 0.1 mg),
Was added to a small beaker containing 2 mL of acetic acid solution and transferred to 1 L brown volumetric flask with a standard concentration of 100 μg/mL.
Preparation of liquid. The standard stock solution is diluted with water to the standard working solution at the appropriate concentration. The stock solution was stored at 4 ° C in the dark. each
6 months to prepare once.
5 instruments and equipment
5.1 Gas chromatograph with mass selective detector.
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 steam distillation unit.
5.4 Centrifuge. 5 000 r/min.
5.5 Rotary Evaporator.
5.6 Oscillator.
5.7 Ultrasonic instrument.
5.8 Solid phase extraction column. silica gel, 6 mL, 1 000 mg, or equivalent.
5.9 Erlenmeyer flask. 250 mL.
5.10 plug test tube. 25 mL.
6 Preparation and storage of samples
6.1 Preparation of the sample
6.1.1 Fruits and vegetables
Take apples, parsley and other representative samples of about 500 g, chopped, with a crusher to sample processed into a slurry. Mix well into a clean capacity
Inside, sealed and marked. -18 ℃ below the preservation.
6.1.2 Grains and nuts
Take about 500 g of representative samples of rice, soybeans, peanuts, etc., crushed with a pulverizer and passed through a 20 mesh round hole. Mix well into the clean
Net inside the container, sealed and marked. 4 ℃ below the preservation.
6.1.3 Animal source food
Take a typical sample of chicken, fish, etc. Approximately 500 g minced with a meat grinder, mix well, fit into a clean container, sealed and marked.
-18 ℃ below the preservation.
6.1.4 honey and tea
Take about 500 g of representative samples of honey and tea, into a clean container, sealed and marked. 4 ℃ below the preservation.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
7. Analysis steps
7.1 Extraction
Grain, Nuts. Weigh the sample 25 g (accurate to 0.1 g) In a 250 mL stoppered Erlenmeyer flask, add 100 mL of water,
Oscillator oscillates for 30 min. Centrifuge at 4 000 r/min for 10 min, pour the supernatant into a distillation flask, add 50 mL of sodium hydroxide solution,
A small amount of water to wash the bottle wall, connect the steam distillation device, slowly heated to boiling. Add 3 mL of acetic acid solution in advance, 25 mL of salicylaldehyde 50 μL
With a plug test tube to receive distillate, collecting distillate about 15 mL.
Vegetables, fruit, aquatic products, muscle tissue, tea, honey. weighed 25 g (accurate to 0.1 g) at 250 mL
Bottle, add 100 mL of water, cover the plug, shaking on the oscillator for 30 min. The extract was poured directly into a distillation flask and the sodium hydroxide solution 50 was added
ML, rinse the bottle with a small amount of water, connect the water vapor distillation unit, slowly heated to boiling. With the addition of acetic acid solution in advance 3 mL, salicylaldehyde 50 μL
Of the 25 mL stopper tube to receive distillate, collecting distillate about 15 mL.
7.2 Derived
The tube was received at 50 ° C for 30 min. After cooling to room temperature, add about 3 g of sodium chloride, 5 mL of n-hexane and shake for 1 min. Static stratification,
The upper n-hexane phase was purified or GC-MS (vegetable, fruit, tea, honey samples were purified by 7.3 and other samples were directly injected).
The appropriate volume of 1,1-dimethylaminide standard solution was derivatized as described above for GC-MS determination.
7.3 purification
For vegetables, fruits, tea, honey samples, with silica gel solid phase extraction column (SPE) purification. The solid phase extraction column was pre-leached with 10 mL of n-hexane
Wash, accurately remove the hexane solution 4 mL to the solid phase extraction column, rinse with 10 mL of n-hexane, and then 5 mL of ethyl acetate n-hexane solution leaching,
10 mL of ethyl acetate n-hexane solution. The eluate was collected and concentrated to dryness under reduced pressure at 50 ° C and set to 4 mL with n-hexane for GC-MS
Determination.
7.4 determination
7.4.1 Gas Chromatography - Mass Spectrometry Reference Conditions
A. Column. DB-5MS quartz capillary column, 30 m × 0.25 mm (inner diameter), film thickness 0.25 μm, or equivalent;
B. Column temperature. 70 ° C 270 ° C (5 min);
C. Inlet temperature. 240 ° C;
D. Chromatography - mass spectrometer interface temperature. 280 ° C;
E. Carrier gas. helium, purity ≥99.995%, 1.0 mL/min;
F Injection volume. 1 μL;
G. Injection method. no split injection, 0.75 min after the valve;
H Ionization mode. EI;
I Ionization energy. 70 eV;
J. Measurement method. Select the ion monitoring mode (SIM);
K Monitoring ions (m/z). quantification 164, qualitative 149,163,165;
L. Solvent delay. 6 min.
7.4.2 Determination and confirmation of chromatography
7.4.2.1 Quantitative determination
According to the content of butyryl hydrazine in the sample solution, the selective concentration of 1,1-dimethyl-labeled standard solution was similar. 1,1-dimethyl
The reaction value of the 1,1-dimethylaminobenzene derivative in the standard solution and the sample solution should be within the linear range of the instrument. The 1,1-
15 ° C/min
Dimethylsilane standard working solution derivatives and sample volumes were measured by volume injection.
Under the above chromatographic conditions, the retention time of 1,1-dimethylaminide derivatives was about 8.17 min. 1,1-dimethylaminide standard derived
The chromatogram of the material SIM is shown in Appendix A, Figure A.1.
7.4.2.2 Gas Chromatography-Mass Spectrum Confirmation
Standard solution derivatives and sample solutions are determined according to the conditions specified in 7.4.1, if the sample solution with the standard solution derivatives of the same retention
Between the emergence of a peak, then its mass spectrometry confirmed. It was confirmed that the retention time of the SIM chromatographic peak was consistent with that of the standard sample,
In addition to the background of the sample spectrum, the selected ions appear; select ion m/z 164, 149,163,165 (its abundance ratio 100. 8. 7. 14)
The relative abundance of the ions associated with the standard sample derivative is consistent and the similarity is within the allowable deviation (see Table 1). 1,1-dimethyl-linked standard
The spectrum of the quasi-derivative SIM is shown in Figure A.2 in Appendix A.
Table 1 GC-MS confirms the maximum allowable deviation of relative ion abundance
7.5 blank test
In addition to the sample, according to the above steps.
8 results are calculated and expressed
Use the chromatographic data processor or calculate the content of butyrylhydrazide in the sample according to formula (1). The calculation result must be deducted from the blank value.
A × c × V × 2.67 (1)
AS x m
Where. X - the content of butyryl hydrazine in the sample, mg/kg;
C - concentration of 1,1-dimethylbisamine derivative in standard working solution in micrograms/ml, μg/mL;
A - the peak area of the 1,1-dimethylbisamine derivative in the sample solution;
AS - the peak area of 1,1-dimethylbisamine derivatives in standard working solutions;
V - the final volume of the sample solution, in milliliters, mL;
M - the amount of sample represented by the final sample, in grams, g;
2.67-- 1,1-dimethyl hydrazine and butyryl hydrazine conversion factor.
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 reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the
Record 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 the
Record the requirements of D.
10% limit and recovery rate
10.1 Quantitation limits
The quantification limit of this method is 0.01 mg/kg.
10.2 Recovery rate
The sample addition concentration and recovery data are given in Appendix B.
Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10%
Allowable relative deviation ± 20% ± 25% ± 30% ± 50%
X =
Appendix A
(Informative)
Standard chromatogram
Figure A.1 1,1-Dimethylaminide Derivative Selective Ion Monitoring Mode (S IM) Total Ion Flow Diagram (T IC)
144 150 156 162 168 174
Figure A.2 1,1-Dimethylaminide Derivative Selective Ion Monitoring Mode (S IM) Mass Spectrometry
1,1-dimethylbisamine derivatives
TR/min
Abundance
Abundance
M/z
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
0.01 mg/kg addition
Recovery rate range (%)
Precision
(RSD%)
0.02 mg/kg add
Recovery rate range (%)
Precision
(RSD%)
0.05 mg/kg add
Recovery rate range (%)
Precision
(RSD%)
Peanut 90.5 100.3 7.8 89.2 95.6 4.6 88.6 92.4 3.4
Rice 91.2100.7 7.0 86.595.6 6.8 86.292.2 3.4
Soybean 90.7 97.8 5.6 91.9 99.8 5.8 87.8 94.4 3.8
Parsley 85.796.2 8.0 81.392.6 6.0 82.790.2 6.4
Apple 84.695.1 7.4 85.695.7 6.6 85.093.2 4.2
Fish 86.794.9 4.8 87.896.7 3.0 90.298.0 3.4
Chicken 88.094.6 4.0 92.397.8 3.8 93.198.2 2.2
Tea 96.0104.7 5.8 97.1 103.5 5.2 98.9 106.8 6.0
Honey 94.3103.7 6.4 80.489.2 6.8 85.492.7 4.8
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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