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GB 23200.82-2016: Food safety national standard -- Determination of ethephon residues in meat and meat products
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Food safety national standard -- Determination of ethephon residues in meat and meat products
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GB 23200.82-2016
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Basic data | Standard ID | GB 23200.82-2016 (GB23200.82-2016) | | Description (Translated English) | Food safety national standard -- Determination of ethephon residues in meat and meat products | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 9,956 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN 0705-1997 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.82-2016: Food safety national standard -- Determination of ethephon residues in meat and meat products
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Food safety national standard - Determination of ethephon residues in meat and meat products
National Standards of People's Republic of China
GB
Instead of SN 0705-1997
National standards for food safety
Determination of ethephon residues in meat and meat products
National food safety standards-
Determination of ethephon residues 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
23200.82-2016
Foreword
This standard replaces SN 0705-1997 "Method for the detection of ethephon residues in meat and meat products for import and export".
This standard compared with SN 0705-1997, 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";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN 0705-1997.
23200.82-2016
National standards for food safety
Determination of ethephon residues in meat and meat products
1 Scope
This standard specifies sample preparation and gas chromatographic methods for the detection of ethephon residues in meat and meat products.
This standard applies to pork, beef, chicken and other residues in the detection of ethephon, 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
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 ethephon residue in the sample is extracted with methanol and the extract is frozen to remove the fat and wax, and then concentrated, and the sample is extracted with ether
And derivatized by diazomethane, the ethephon derivative derived from dimethyl ethephon, with a nitrogen and phosphorus detector with gas chromatography, 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 Potassium hydroxide (KOH). Analytical purity.
4.1.2 Methanol (CH3OH). Distillation.
4.1.3 N-methyl-N-nitroso-p-toluenesulfonamide (C8H10N2O3S).
4.1.4 anhydrous ethanol (CH3CH2OH).
4.1.5 anhydrous ether. (C4H10O). re-distillation.
4.1.6 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, placed in a sealed container in reserve.
4.2 solution preparation
4.2.1 Methanol - Hydrochloric acid (38%) solution (90 10).
4.2.2 Diazomethane solution. 10 ml of aqueous solution of potassium hydroxide (0.6 g/mL), 35 mL of ethanol and 10 mL of ether
The double mouth distilled bottle is placed in a water bath on a magnetic stirrer heating plate. Place the stir bar in the bottle, connect the dropping funnel and the high-performance condenser, and condense it
After the series, two 125 mL flasks were used as receiving bottles. 10 mL of ether was placed in the second flask and the inlet tube was inserted into the ether level
the following. Place the two receiving bottles in an ice bath. The water bath was heated to 70 ° C while stirring with a magnetic stirrer and dropping from the dropping funnel
A solution of N-methyl-N-nitroso-p-toluenesulfonamide in diethyl ether (21.5 g/140 mL) was added. The time to complete the total solution was controlled at 20 min
, When the distillate was pale yellow, stop the distillation. The liquids in the two receiving bottles were combined as a diazomethane solution. If it contains impurities too
Can be re-distilled. The solution is stored in a refrigerator and stored for one month.
4.3 standards
4.3.1 ethephon standard. purity ≥ 99%
4.4 standard solution preparation
4.4.1 ethephon standard solution. accurately weighed the right amount of ethephon standard, with methanol prepared into a concentration of 1.0 mg/mL standard reserve
Liquid, dilute the standard stock solution with methanol to prepare the standard working solution at the appropriate concentration. Note. should be used when preparing standard solutions
Polyethyleneware.
5 instruments and equipment
5.1 Gas chromatography with nitrogen and phosphorus detector.
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 Quick Mixer.
23200.82-2016
5.4 Centrifuge. 6000 r/min.
5.5 Polyethylene flask. 100 mL with stopper.
5.6 Polyethylene beaker. 250 mL.
5.7 Microinjector. 10 μL or 5 μL.
5.8 Ultrasonic bath.
6 Analysis steps
6.1 Extraction
Weigh about 20 g of sample (accurate to 0.1 g) in a polyethylene beaker by adding 0.5 mL of methanol-hydrochloric acid (90 10) solution and 40 mL of methanol,
Extraction in an ultrasonic bath for 5 min. After centrifugation in a centrifuge tube (6000 r/min) for 2 min, the supernatant was aspirated with 100 mL of polyethylene
In a polyethylene flask. The residue was again extracted with 40 mL of methanol as described above and the combined extracts were pooled in the same polyethylene flask.
6.2 purification
The polyethylene flask containing the methanol extract was frozen in a freezer at -18 ° C for 4 h. Removed quickly after the transfer into the centrifuge tube
Heart (6000 r/min) 5 min. The supernatant was poured into a 250 mL heart flask treated with dimethyldichlorosilane. The remaining residue was washed with 2 mL
Frozen methanol washed, the lotion transferred to the same heart bottle. Concentrated to about 60 mL on a 30-35 & lt; 0 & gt; C water bath with a rotary evaporator. Will be thick
The distillate was transferred to a 100 mL volumetric flask treated with dimethyldichlorosilane. Wash the flask with a small amount of methanol, the lotion into the volumetric flask.
With methanol volume.
6.3 Derivatization
10.0 mL of the above solution was taken, placed in a 15 mL stoppered centrifuge tube, and concentrated in a 30-35 ° C water bath under a dry nitrogen stream
About 1.5 mL. Add 0.5 mL of methanol-hydrochloric acid solution (90 10) and 8 mL of anhydrous ether, mix well for 10 min. Will be the upper layer
The solution was poured into another plug tube and the residue was washed with 2 x 1 mL of anhydrous ether. The lotion is incorporated into the above solution. Under nitrogen flow
30-35 ° C water bath to about 1 mL. In the fume hood, dropping the diazomethane solution into the concentrate until the yellow does not fade. Cover strict
Stopper, placed for 15 min. The excess diazomethane was blown off with a nitrogen stream. And then washed with 2 × 5 mL water, each centrifugation (6000 r/min) 2 min,
Discard the lower aqueous phase. Concentrate to about 0.8 mL in a 30-35 ° C water bath with a nitrogen stream and dilute to 1.00 mL with anhydrous ether. The solution is treated with about
0.5 g anhydrous sodium sulfate after dehydration gas chromatographic determination.
6.4 Derivation of standard solutions
Take the appropriate amount of ethephon standard working solution, placed in a 100 mL stoppered polyethylene flask, add diazomethane solution until yellow does not fade
until. Cover the stopper and place it for 15 min. The excess diazomethane was blown off with a nitrogen stream, and the solution became colorless. The flask was placed at 30-35 ° C
The water bath was concentrated to near dryness under a nitrogen stream and the residue was dissolved in anhydrous ether and diluted to the same volume of the standard working solution.
6.5 Determination
6.5.1 Gas Chromatographic Reference Conditions
A) Column. stainless steel column, 2m × 3 mm (inner diameter), filler 3% (m/m) FFAP applied to Chromosorb G, AW,
DMCS (60-80 mesh);
B) Carrier gas. nitrogen, purity ≥ 99.9%, 50 mL/min
C) Hydrogen. 4 mL/min ;.
D) Air. 175 mL/min
E) Column temperature. 145 ° C
F) Inlet temperature. 230 ° C
G) Detector temperature. 300 ° C
H) Injection volume. 1 μL
6.5.2 Chromatographic determination and confirmation
According to the sample measured pesticide content, selected peak height similar to the standard working solution, the standard working solution and the sample solution of pesticides
The response value of the derivative should be within the linear range of the instrument detection. The standard solution and the sample solution should be equal to the volume of the sample injection. In the above color
Under the conditions of the spectrum, the retention time of the ethephon derivative (dimethyl ethenanthrene) was about 1.6 min. The chromatograms of the standard derivatives are shown in Appendix A.
Figure A1.
6.6 blank experiment
Unless the sample is not weighed, according to the above measurement steps.
7 Results calculation and presentation
Use the chromatographic data processor or calculate the content of each benzamide pesticide in the sample according to the following formula.
23200.82-2016
Mh
Vch
Where.
X - Residual content of ethephon in sample, mg/kg;
H - the chromatographic peak of dimethyl ethenanthrene in the sample solution, mm;
Hs - standard working solution of dimethyl vinyl chloride peak height, mm;
C - the concentration of ethephon in standard working fluid, μg/mL;
V - the final volume of the sample solution, mL;
M - the amount of sample represented by the final sample, 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.
8 precision
8.1 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.
8.2 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.
9 Quantitation limit and recovery rate
9.1 Limit of limits
The limit of gelatinization of this method is 0.01 mg/kg.
9.2 Recovery
When the addition level was 0.01 mg/kg, 0.1 mg/kg, 1 mg/kg, the recovery rate of ethephon was 84.6-90.2%.
23200.82-2016
Appendix A
(Suggested appendix)
Standard chromatogram
Figure A1 Derivatives of ethephon standard (dimethyl ethenanthrene) Gas chromatogram
23200.82-2016
Appendix B
(Normative appendix)
Laboratory repeatability requirements
Table B.1 Laboratory repeatability requirements
Measured component content
Mg/kg
Precision
0.001 36
> 0.01
> 1 14
23200.82-2016
Appendix C
(Normative appendix)
Inter-laboratory reproducibility requirements
Table C.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
Precision
0.001 54
> 0.01
> 1 19
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