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GB 23200.80-2016: Food safety national standard -- Determination of Dithiophos Residue in Meat and Meat Products
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Food safety national standard -- Determination of Dithiophos Residue in Meat and Meat Products
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GB 23200.80-2016
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Basic data | Standard ID | GB 23200.80-2016 (GB23200.80-2016) | | Description (Translated English) | Food safety national standard -- Determination of Dithiophos Residue in Meat and Meat Products | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 9,966 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 0709-2012 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.80-2016: Food safety national standard -- Determination of Dithiophos Residue in Meat and Meat Products
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Food safety national standard - Determination of Dithiophos Residue in Meat and Meat Products
National Standards of People's Republic of China
GB
Replace SN/T 0709-2012
National standards for food safety
Determination of Dithiophos Residue in Meat and Meat Products
National food safety standards-
Determination of temephos residue in meats and meat products
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 0709-1997 "Method for the determination of dithiophos residues in meat and meat products".
Compared with SN 0709-1997, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the name of the "export of meat and meat products" to "meat and meat products";
- "Other food can be referred to in the standard range";
- the sampling step was removed;
- homemade Florian column to commercial column.
This standard replaced the previous version of the standard release.
-SN 0709-1997.
National standards for food safety
Determination of the content of dithiophos in meat and meat products
1 Scope
This standard specifies the method for the determination of dithiophos in meat and meat products by gas chromatography-mass spectrometry.
This standard applies to the determination of the amount of dithiophos in export pork, and other foodstuffs can be used for reference.
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
file. 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 residual bisulfophosphamide in the sample was extracted with acetonitrile-methanol mixture (4 1, v/v), the extract was extracted with chloroform,
Shrink to dry, the residue was dissolved with n-hexane, the solution was purified by florisil silica column. Eluting with a mixture of ethyl acetate-n-hexane (3 7, v/v)
The eluate was concentrated and quantified with n-hexane. The solution was subjected to gas chromatography-mass spectrometry and quantified by external standard method.
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 acetonitrile (C2H3N). pesticide residues.
4.1.2 Methanol (CH3O). Pesticide level.
4.1.3 Trichloromethane (CHCl3). Pesticide level.
4.1.4 ethyl acetate (C4H8O2). pesticide residues.
4.1.5 n-Hexane (C6H14). Pesticide level.
4.1.6 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, stored in a sealed container after cooling and standby.
4.2 solution preparation
4.2.1 Sodium Sulfate Solution. 5% aqueous solution.
4.2.2 acetonitrile - methanol mixture (4 1, v/v). take 400 mL of acetonitrile, add 100 mL of methanol, shake back.
4.2.3 Ethyl acetate-n-hexane mixture (3 7, v/v). Take 300 mL of ethyl acetate, add 700 mL of n-hexane and shake well.
4.3 standards
4.3.1 Sulfophosphate standard substance. purity ≥98.0%
4.4 standard solution preparation
4.4.1 Dithiophosphoric acid standard solution. accurately weighed the appropriate amount of bisphosphorus standard, with a small amount of benzene dissolved, and then with n-hexane prepared into the concentration of
2.0 mg/mL standard stock solution, stored in the refrigerator. If necessary, dilute with n-hexane to the standard working solution at the appropriate concentration.
4.5 Materials
4.5.1 Florisil Column. 4 g.
5 instruments and equipment
5.1 Gas Chromatography-Mass Spectrometer, with electron bombardment ion source (EI source).
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 Centrifuge.
5.4 Crusher.
5.5 Rotary evaporator.
5.6 Microiner. 10 μL.
5.7 Oscillator.
6 Preparation and storage of samples
6.1 Preparation of the sample
To replace the sample of about 1000 g, crushed by grinding, mixing, are divided into two, respectively, into the clean container as a sample, sealed,
And mark the mark.
6.2 Sample storage
The sample was stored at -18 ° C or lower. During the operation of the sample preparation, it is necessary to prevent contamination of the sample or change in the content of the residue.
7 Analysis steps
7.1 Extraction
Weigh about 10 g of sample (accurate to 0.1 g) in a conical flask and add 50 mL of acetonitrile-methanol mixture (4 1, v/v) for 30 min.
Centrifuge at 4000 rpm for 15 min, remove the supernatant in a separatory funnel. And then three times with 3 × 25 mL methanol washing the sample three times, wash with the former
The supernatant was combined in the same separatory funnel.
7.2 Purification
In the above-mentioned separatory funnel by adding 100 mL of sodium sulfate aqueous solution and 50 mL of chloroform, shaking 5 min, standing stratification, the next
The layer of the chloroform solution was introduced into a flask through a funnel containing anhydrous sodium sulfate. And then separately with 50 mL of chloroform extraction twice, combined with trichloride
V - the total volume after dilution of the sample in liters (L);
M - sample mass 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 B 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 C requirements.
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 addition level is in the range of 0.1 ~ 1.0 mg/kg, the recovery of dithiophosphate is 83.6% ~ 103.2%.
Appendix A
(Informative)
Spectrum of bisulfophosphate standard solution
4 .0 06.08.00 01.00 01.2.01.4006.60.08.80.00.00
T ime - - >
A bundance
TIC. STD 1 1 .D \\ data .ms
1 8 .0 1 2
Figure A.1 Total ion chromatogram of bisulfophosphate standard solution
5 0 1 0 0 1 5 0 2 0 0 2 5 0 3 0 0 3 5 0 4 0 0 4 5 0 5 0 0
M/z - - >
A bundance
A verageof 1 9 .7 5 5 to 1 9 .8 0 8 m in.. TEMESTD 3 .D \\ DATA .MS (-)
2 3 1 4 3 43 7 22 6 36 9 3 1 3 4 0 32 9 31 4 7 5 0 3
Figure A.2 Total sweep mass spectra of bisulfophosphate standard solutions
Appendix B
(Normative appendix)
Laboratory repeatability requirements
Table B.1 Laboratory repeatability requirements
Measured component content
Mg/kg
RSD
0.001 36
> 0.01
> 1 14
Appendix C
(Normative appendix)
Inter-laboratory reproducibility requirements
Table C.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
RSD
0.001 54
> 0.01
> 1 19
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