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GB 23200.68-2016: Food safety national standard -- Determination of residues of pyridine residues in food by gas chromatography-mass spectrometry
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Food safety national standard -- Determination of residues of pyridine residues in food by gas chromatography-mass spectrometry
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GB 23200.68-2016
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Basic data | Standard ID | GB 23200.68-2016 (GB23200.68-2016) | | Description (Translated English) | Food safety national standard -- Determination of residues of pyridine residues in food by gas chromatography-mass spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 11,111 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 2648-2010 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.68-2016: Food safety national standard -- Determination of residues of pyridine residues in food by gas chromatography-mass spectrometry
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Food safety national standards - Determination of residues of pyridine residues in food by gas chromatography - mass spectrometry
Replace SN/T 2648-2010
National standards for food safety
Determination of Residual Potassium Amide Residues in Foods
Gas chromatography - mass spectrometry
National food safety standards-
Determination of boscalid residue in foods
Gas chromatography-mass spectrometry
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
GB
National Standards of People's Republic of China
Foreword
This standard replaces SN/T 2648-2010 "Determination of the residual amount of pyridine amines in the import and export food by gas chromatography-mass spectrometry".
Compared with SN/T 2648-2010, 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 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 2648-2010.
National standards for food safety
Determination of residues of pyridine residues in food by gas chromatography - mass spectrometry
1 Scope
This standard specifies the method for the determination of pyridine residues in food by gas chromatography-mass spectrometry.
This standard applies to spinach, carrots, strawberries, peanuts, chestnuts, tea, onions, chicken, cod and honey in the residual
The amount of detection and confirmation; 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 date of the note applies
This document. 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 solution was extracted with acetonitrile and purified by liquid/liquid distribution and propyl ethylenediamine bonded silica gel (PSA) solid phase extraction column.
Gas chromatography - electron bombardment mass spectrometry, external standard method.
4 reagents and materials
Unless otherwise specified, the reagents used are of analytical grade and the water is in accordance with the primary water specified in GB/T 6682.
4.1 Reagents
4.1.1 Acetone (C3H6O). Pesticide Residue.
4.1.2 acetonitrile (C2H3N). pesticide residues.
4.1.3 N-Hexane (C6H14). Pesticide Residue.
4.1.4 sodium chloride (NaCl). 650 ℃ burning 4 h, placed in a dryer cooling, standby.
4.2 solution preparation
4.2.1 n-hexane saturated acetonitrile. take 100mL n-hexane, 100mL acetonitrile in the separatory funnel, shake and mix, take the next stand.
4.2.2 acetonitrile saturated n-hexane. take 100mL n-hexane, 100mL acetonitrile in the separatory funnel, the oscillation mix, take the upper stand.
4.2.3 Acetone-n-Hexane (3 7, v/v). Take 300 mL of acetone, add 700 mL of n-hexane and shake well.
4.3 standards
4.3.1 pyridinamide standard substance (boscalid, CAS No. 188425-85-6, molecular formula. C18H12Cl2N2O). purity ≥ 98.0%.
4.4 standard solution preparation
4.4.1 Dipyridine standard solution. accurately weighed the appropriate standard with acetone dissolved and prepared into a standard concentration of 1.0 mg/mL reserve
liquid. According to the need to use pyridine-free blank sample matrix solution diluted to the appropriate concentration of standard working solution. Store at -18 ° C
In the refrigerator.
4.5 Materials
4.5.1 Primary secondary amine (PSA) solid phase extraction column. 500 mg, 3 mL or equivalent.
5 instruments and equipment
5.1 Gas Chromatography-Mass Spectrometer. Equipped with an electron impact source (EI).
5.2 solid phase extraction device.
5.3 homogenizer, speed 10000 r/min.
5.4 Rotary Evaporator.
5.5 nitrogen concentrator.
5.6 with a plug centrifuge tube. 50 mL, 100 mL.
5.7 Concentrated bottles. 50 mL, 100 mL.
5.8 Analytical balance. 0.01 g and 0.0001 g.
6 Preparation and storage of samples
6.1 Preparation of the sample
6.1.1 Grains and nuts
Take a representative sample volume of 500g, all ground and pass through a 2.0 mm round hole screen. Mix well, into a clean container, sealed,
Mark the mark.
6.1.2 Fruits and vegetables
Take a representative sample 500g, chopped (not washable), with a food mashed machine to sample into a slurry. Mix well and put it clean
Of the container, sealed, marked mark.
6.1.3 Meat and fish
Take a representative sample 500g, fully crushed evenly, into a clean container as a sample. Sealed, marked.
6.1.4 honey
Take a representative sample 500g, the crystallization of honey samples will be evenly stirred; on the crystallization of honey samples, in the closed
The case, the sample bottle placed in not more than 60 ℃ in the water bath in the warm, shaking, until the sample all melted and stir well, quickly cooled to room temperature,
In the melting must pay attention to prevent moisture evaporation. Load a clean container, sealed, marked with a mark.
6.1.5 Tea
Take a representative sample of 500 g, grind all with an attritor and pass through a 2.0 mm round hole screen. Mix well and clean the clean container
Inside, sealed, marked mark.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
6.2 Sample storage
Grains and nuts are stored at 0 to 4 ° C; other samples are cryopreserved at -18 ° C or lower.
During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue.
7 measurement steps
7.1 Extraction
Weigh 10 g of sample (accurate to 0.01 g) in a 100 mL stoppered centrifuge tube, add 10 mL of water, add 40.0 mL
Hexane saturated acetonitrile, homogenizer extraction 2 min (honey need to add water 10mL and acetonitrile violent oscillation 20min), then add 5g sodium chloride,
Severe oscillation 10min, 3000 r/min centrifugal 10min, to be purified.
7.2 Purification
7.2.1 Liquid/liquid distribution purification
Take the upper extract 20.0 mL (spinach, carrot, strawberry) or 10.0 mL (peanuts, chicken, onions, cod, honey, chestnut
And tea) were transferred to a 50 mL stoppered centrifuge tube, 10 mL of acetonitrile was added to the saturated n-hexane, shaken for 3 min, left to stand, discarded
The n-hexane phase was removed and the n-hexane phase was discarded again with 10 mL of acetonitrile saturated n-hexane. The lower acetonitrile phase was collected in 100 mL
Concentrated in a 40 ° C water bath and concentrated to approximately 1 mL.
7.2.2 Solid phase extraction (SPE) purification
The PSA column was pre-leached with 5 mL of acetone-n-hexane. The sample solution was poured into the column and eluted with 10 mL of acetone-n-hexane to control the flow rate
At 2 mL/min. The whole eluate was collected and concentrated to near dryness in a water bath at 40 ° C. Dissolved with acetone - n - hexane and set to
1.0 mL, determined by gas chromatography-mass spectrometry.
7.3 Determination
7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions
A) Column. HP-5 MS quartz capillary column, 30 m × 0.25 mm (id), film thickness 0.25 μm, or equivalent;
B) column temperature. the initial temperature of 70 ℃, keep 2 min, 25 ℃/min program temperature to 150 ℃, to 15 ℃/min
The temperature was raised to.200 ° C, and then the temperature was raised to 280 ° C at 10 ° C/min for 10 min.
C) Inlet temperature. 250 ° C;
D) chromatographic - mass spectrometer interface temperature. 280 ° C;
E) Carrier gas. helium, purity greater than or equal to 99.999%, constant current mode, 1mL/min;
F) Injection volume. 1 μL;
G) Injection method. no split injection, 0.65 min after the opening valve;
H) ionization mode. electron bombardment
I) ion source temperature. 230 ° C;
J) quadrupole temperature. 150 ° C;
L) Determination of the way. select the ion monitoring mode;
M) Select the monitoring ion (m/z). Quantitative 140, Qualitative 112, 167, 342;
N) solvent delay. 4.0 min.
7.3.2 Determination and confirmation of chromatography
According to the content of the sample in the sample, select the concentration of similar matrix standard working solution, the standard working solution and sample solution
The response value of the solution in the matrix standard working solution and the sample solution to be measured should be within the linear range of the instrument detection.
If the sample solution is in the selective ion chromatogram of the standard working solution, a chromatographic peak appears at the same retention time,
In the sample quality chromatogram, the selected ions are present, the abundance of the selected ions is greater than the abundance ratio of the corresponding ions
Within the allowable range (see Table 1). Under the above chromatographic conditions, the retention time of pyridine amines was about 18.8 min, and the monitored ions (m/z)
Which was confirmed by m/z 140, 112, 167, 342 (the relative abundance ratio was 100. 33. 13. 27); according to the quantitative ion m/z140
The amount of its external standard method. The chromatographic total ion chromatogram and full scan of the acridine amide standard under the above chromatographic conditions
The spectra are shown in Appendix A, Figures A.1 and A.2.
Table 1 confirms the maximum allowable error of relative ion abundance
Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10%
Allowable relative deviation ± 20% ± 25% ± 30% ± 50%
7.4 blank test
In addition to the sample, according to the above steps.
8 results are calculated and expressed
Use the chromatographic data processor or (1) to calculate the residual amount of pyridylamine in the sample.
H × c × V
X = ------------------------------. (1)
Hs × m
Where.
X - the residual amount of pyridylamine in the test, in milligrams per kilogram (mg/kg);
H - the peak of the chromatographic peak of pyridinamide in the sample solution;
C - the concentration of pectin in standard working solution, in micrograms per milliliter (μg/mL);
V - the final volume of the sample solution in milliliters (mL);
Hs - the peak of the chromatographic peak of pyridinamide in standard working solution;
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)
Together with the requirements of Appendix C.
9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage)
Together with the requirements of Appendix D.
10% limit and recovery rate
10.1 Quantitation limits
The limit of quantification of the method is 0.1 mg/kg.
10.2 Recovery rate
When the levels were 0.01 mg/kg, 0.02 mg/kg, 0.04 mg/kg, the addition of pyridinamines was given in Appendix B.
Appendix A
(Informative)
Total Ion Flow Chromatogram and Mass Spectrometry of Pyridinoside Standard Substance
Figure A.11 Total ion chromatogram of pyridinamide standard
Figure A.2 Chromatogram of Pyridinoside Reference Substance
Appendix B
(Informative)
Sample concentration and recovery range of experimental data
Table B.1 Experimental data on sample concentration and recovery range
sample
Add concentration
(Mg/kg)
Recovery rate range (%) sample
Add concentration
(Mg/kg)
Recovery rate range (%)
spinach
0.01 90.0 to 110.0
Codfish
0.01 90.0 to 110.0
0.02 97.5 to 112.5 0.02 97.5 to 104.5
0.04 95.0 to 105.0 0.04 94.0 to 112.0
carrot
0.01 95.0 to 111.0
honey
0.01 90.0 to 110.0
0.02 95.0 to 107.0 0.02 92.5 to 102.5
0.04 96.0 to 105.0 0.04 95.0 to 105.0
Strawberry
0.01 95.0 to 110.0
Chestnut
0.01 95.0 to 110.0
0.02 97.5 to 105.5 0.02 92.5 to 107.5
0.04 97.0 to 105.0 0.04 95.0 to 106.0
peanut
0.01 90.0 to 110.0
tea
0.01 90.0 to 110.0
0.02 97.5 to 107.5 0.02 97.5 to 112.5
0.04 98.0 to 107.0 0.04 98.05 to 103.0
chicken
0.01 95.0 to 110.0
0.01 95.0 to 110.0
0.02 96.0 to 107.5 0.02 97.5 to 105.0
0.04 94.0 to 106.0 0.04 95.0 to 112.0
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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