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GB 23200.79-2016: Food safety national standard -- Meat and meat products -- Determination of mycophenolate residues -- Gas chromatographic method
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Food safety national standard -- Meat and meat products -- Determination of mycophenolate residues -- Gas chromatographic method
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GB 23200.79-2016
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Basic data | Standard ID | GB 23200.79-2016 (GB23200.79-2016) | | Description (Translated English) | Food safety national standard -- Meat and meat products -- Determination of mycophenolate residues -- Gas chromatographic method | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 10,115 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 0675-2011 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.79-2016: Food safety national standard -- Meat and meat products -- Determination of mycophenolate residues -- Gas chromatographic method
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Food safety national standard - Meat and meat products - Determination of mycophenolate residues - Gas chromatographic method
National Standards of People's Republic of China
GB
Instead of SN/T 0675-2011
National standards for food safety
Determination of mycophenolate residues in meat and meat products
Gas chromatography
National food safety standards-
Determination of pyrazophos residue in meat 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
Ministry of Agriculture of the People 's Republic of China
State Administration of Food and Drug Administration
release
Foreword
This standard replaces SN/T 0675-2011 "Gas Chromatography" for the determination of bacteria and phosphorus residues in meat and meat products.
This standard compared with SN/T 0675-2011, 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 "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/T 0675-2011.
National standards for food safety
Meat and meat products - Determination of mycophenolate residues - Gas chromatographic method
1 Scope
This standard specifies the method for the determination of mycophenol residues in meat and meat products by gas chromatography.
This standard applies to pork, chicken and beef in the determination of the residual amount of mycobacterial phosphorus, 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 extracted with cyclohexane-ethyl acetate (1 + 1, volume ratio). The extract was purified by gel permeation chromatography,
Determination by gas chromatography, external standard method quantitative.
4 reagents and materials
Unless otherwise specified, the reagents used are analytically pure and water is the primary water specified in GB/T 6682.
4.1 Reagents
4.1.1 Cyclohexane (C6H12). Chromatographic Purification.
4.1.2 Ethyl acetate (C4H8O2). Chromatographic purity.
4.1.3 n-hexane (C6H14). chromatographic purity.
4.1.4 Toluene (C7H8). Chromatographic pure.
4.1.5 anhydrous sodium sulfate (Na2SO4). before burning at 650 ℃ for 4 h, stored in a dryer, cooling and standby.
4.2 solution preparation
4.2.1 Cyclohexane-ethyl acetate mixed solvent (1 +1, volume ratio). take 100mL cyclohexane, add 100mL ethyl acetate, shake
Evenly used.
4.3 standards
4.3.1 Pythium Phosphate standard substance (pyrazophos; formula. C14H20N3O5PS; CAS No. 13457-18-6). purity ≥97%.
4.4 standard solution preparation
4.4.1 Pythium phosphate standard stock solution. accurately weighed appropriate amount of Pseudomonas citrate standard substance (accurate to 0.1 mg), with toluene concentration of about
A standard stock solution of 1.0 mg/mL.
4.4.2 Pythium standard working solution. According to the testing requirements, respectively, the above standard stock solution diluted with n-hexane diluted to the appropriate concentration of the standard
Quasi-working solution.
4.5 Materials
4.5.1 Filtration. 0.45 μm, organic.
4.5.2 anhydrous sodium sulfate column. in the cylindrical funnel (diameter 1.5 cm), containing about 5 cm high anhydrous sodium sulfate.
5 instruments and equipment
5.1 Gas Chromatograph. with flame photometric detector (FPD), with a phosphorus filter.
5.2 Gel Permeation Chromatography.
5.3 Analysis of balance. 0.01 g and 0.0001 g.
5.4 Centrifuge.
5.5 Rotary Evaporator.
5.6 nitrogen dryers.
5.7 homogenizer.
6 Sample preparation and storage
6.1 Preparation of the sample
Sampling parts according to GB 2763 Appendix A implementation, the sample with meat grinder minced, fully mixed, with a quarter to shrink to less than 500 g, installed
Into the clean container, sealed, marked mark.
6.2 Storage of samples
The sample was stored at -18 ° C or lower.
7 Analysis steps
7.1 Extraction
Weigh 10 g of sample (accurate to 0.01 g) in a 100 mL centrifuge tube containing 20 g of anhydrous sodium sulfate, add 30 mL of cyclohexane-acetic acid
Ethyl ester mixed solvent, homogenized at 15 000 r/min homogeneous extraction 1.5 min, centrifuged at 3000 r/min for 3 min. Supernatant is filled with
An anhydrous sodium sulfate canister was collected in 100 mL pear bottles. The residue was extracted with 30 mL of cyclohexane-ethyl acetate mixed solvent
The combined extracts were washed twice and the anhydrous sodium sulphate column was washed with a small amount of cyclohexane-ethyl acetate mixed solvent. The extract was washed with water at 40 ° C
Turn to about 2 mL, to be purified.
7.2 Purification
7.2.1 Gel Permeation Chromatography Instrument Conditions
A) Purification column. 400 mm × 25 mm, built with BIO-Beads S-X3 packing or equivalent.
B) Mobile phase. cyclohexane-ethyl acetate (1 + 1, volume ratio).
C) Flow rate. 5 mL/min.
D) Injection volume. 5 mL.
E) Start collection time. 1.200 s.
F) End of collection time. 1 800 s.
7.2.2 Purification steps
The concentrated extract was transferred to a 10 mL graduated centrifuge tube and washed several times with a cyclohexane-ethyl acetate mixed solvent.
And wash the liquid and constant volume to the scale. After centrifugation at 4 000 r/min for 5 min, the supernatant was filtered through a 0.45 μm organic phase filter into a gel permeation chromatograph
In the sample bottle. Purified with a gel permeation chromatograph and collected effluent from 1.200 s to 1 800 s. The effluent was dried with a nitrogen dry drier and added
1.0 mL n-hexane dissolved, mixed, gas chromatographic determination.
7.3 Determination
7.3.1 Chromatographic determination of reference conditions
A) Column. HP-5, 30 m x 0.32 mm (id), film thickness 0.25 μm, or equivalent.
B) column temperature. initial temperature 220 ℃, keep 10 min; at 10 ℃/min rate rose to 250 ℃, keep 7 min.
C) Carrier gas (N2). 1.5 mL/min.
D) Hydrogen (H2). 75 mL/min.
E) Air. 100 mL/min.
F) Detector temperature. 280 ° C.
G) Inlet temperature. 250 ° C.
H) Injection volume. 1 μL.
I) Injection method. no split injection, 1.5 min after opening the diverter valve.
7.3.2 Chromatographic determination
According to the content of mycorrhizal phosphorus in the sample, select the appropriate concentration of the standard working solution and the sample to be measured and other volume injection. Standard working fluid and pending
The response value of the mycophenolate in the sample solution should be within the linear range of the instrument response. Under the above chromatographic conditions, the retention time of mycorrhizal phosphorus is about 14.9
Min, according to the peak area external standard method. See Appendix A for standard chromatograms.
7.4 blank test
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 residual content of mycophenolate in the sample.
MA
VcA
. (1)
Where.
X - Residual content of mycophenolate in the sample, in milligrams per kilogram (mg/kg);
A - the peak area of the pyrrole peak in the sample solution;
Cs - the concentration of mycophenolate in standard working solution in micrograms per milliliter (g/mL);
V - the final volume of the sample solution in milliliters (mL);
AS - peak area of pyrophosphate peak 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) 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 quantification limit of this method is 0.01 mg/kg.
10.2 Recovery rate
When the levels were 0.01 mg/kg, 0.02 mg/kg, 0.05 mg/kg, the recovery of the mycophenolate was given in Appendix B.
Appendix A
(Informative)
Pseudomonas aeruginosa standard gas chromatogram
Figure A.1 Pyridine phosphorus standard gas chromatogram
Appendix B
(Informative)
Table B.1 Recovery and precision of the three matrix samples
Substrate Name Added Level/(mg/kg) Recovery Range/(%) Precision/RSD (%)
pork
0.01 82.5 to 104.2 8.3
0.02 82.1 to 96.7 5.6
0.05 83.5 to 93.1 3.9
chicken
0.01 80.8 to 103.3 8.0
0.02 80.0 to 92.5 5.2
0.05 80.8 to 96.5 5.9
beef
0.01 81.7 to 107.5 8.0
0.02 83.8 to 97.5 5.8
0.05 82.7 to 97.7 5.9
Appendix C
(Normative appendix)
Laboratory repeatability requirements
Table C.1 Laboratory repeatability requirements
Measured component content
Mg/kg
RSD
0.001 36
> 0.01
> 1 14
Appendix D
(Normative appendix)
Inter-laboratory repeatability requirements
Table D.1 Inter-laboratory repeatability requirements
Measured component content
Mg/kg
RSD
0.001 54
> 0.01
> 1 19
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