|
US$179.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email.
GB 23200.97-2016: Food safety national standard -- Determination of 5 organophosphorus pesticide residues in honey -- Gas chromatographic method
Status: Valid
| Standard ID | Contents [version] | USD | STEP2 | [PDF] delivered in | Standard Title (Description) | Status | PDF |
| GB 23200.97-2016 | English | 179 |
Add to Cart
|
3 days [Need to translate]
|
Food safety national standard -- Determination of 5 organophosphorus pesticide residues in honey -- Gas chromatographic method
| Valid |
GB 23200.97-2016
|
PDF similar to GB 23200.97-2016
Basic data | Standard ID | GB 23200.97-2016 (GB23200.97-2016) | | Description (Translated English) | Food safety national standard -- Determination of 5 organophosphorus pesticide residues in honey -- Gas chromatographic method | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 9,936 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 1593-2005 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.97-2016: Food safety national standard -- Determination of 5 organophosphorus pesticide residues in honey -- Gas chromatographic method
---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Food safety national standard - Determination of 5 organophosphorus pesticide residues in honey - Gas chromatographic method
National Standards of People's Republic of China
GB
Instead of SN/T 1593-2005
National standards for food safety
Determination of 5 Organophosphorus Pesticide Residues in Honey
Gas chromatography
National food safety standards-
Determination of five organophosphorus pesticides residues in honey
Gas chromatography
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/T 1593-2005 "five kinds of organophosphorus pesticide residues in the import and export of honey - Gas Chromatography".
Compared with SN/T 1593-2005, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the standard name "import and export of honey" to "honey";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 2572-2010.
National standards for food safety
Determination of 5 organophosphorus pesticide residues in honey - Gas chromatographic method
1 Scope
This standard specifies the determination of trichlorfon, dolphin, chlorpyrifos, malathion, and phosphotoxic pesticide residues in honey by gas chromatography
method.
This standard is applicable to the determination and confirmation of trichlorfon, dolphin, chlorpyrifos, malathion and phosphotoxic pesticide residues in 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
After the honey was diluted with water, the organophosphorus pesticide in the sample was extracted with ethyl acetate, concentrated at low temperature, and the gas phase was measured with a flame photometric detector
Determination of spectrometer, 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 Ethyl acetate (C4H8O2). Chromatographic purity.
4.1.2 Sodium chloride (NaCl).
4.2 standards
4.2.1 Organophosphorus standards. trichlorphon (CAS. 52-68-6), dolphin (fenchlorphos, CAS. 299-84-3),
Chlorpyrifos, CAS. 2921-88-2, malathion, CAS. 121-75-5, coumaphos,
CAS. 56-72-4) with a purity of & gt; 97%.
4.3 standard solution preparation
4.3.1 trichlorfon, dolphin phosphorus, chlorpyrifos, malathion, fly poison phosphorus standard stock solution. were weighed the appropriate standard, respectively, with B
The ethyl acetate was dissolved in a volume of 100 mL and the solution concentration was 100 μl/mL and stored in a 4 ° C refrigerator. Before use, dilute with ethyl acetate as needed
To the appropriate concentration, as a mixed standard working fluid.
5 instruments and equipment
5.1 Gas Chromatograph with Flame Photometric Detector (Phosphor Filter 525 nm).
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 Rotary Evaporator.
5.4 Centrifuge. 4 000 r/min.
5.5 Mixer.
6 Preparation and storage of samples
Stirring of the un-crystallized sample is carried out evenly, and the sampling site is carried out according to GB 2763 Appendix A. For samples with crystalline precipitates,
After the cap is tightened, it is warmed in a water bath that does not exceed 60 ° C. Once the sample has melted and stirred, it is rapidly cooled to room temperature. Must be thawed
Pay attention to prevent moisture from evaporation. The prepared samples were divided into two separate sections, sealed into the vials, sealed and marked.
During the operation of the sample preparation, the contamination of the sample or the change in the content of the residue should be prevented. Store the sample at room temperature.
7 Analysis steps
7.1 Extraction
Weigh 10 g homogeneous sample (accurate to 0.01 g), placed in 50 mL centrifuge tube, add 15 mL of water and 5 g of sodium chloride, mix,
Then add 15 mL of ethyl acetate, mix on the mixer for 2 min, centrifuge 5 min (3 000 r/min), with a pointed nozzle to the upper layer of acetic acid
The ethyl ester solution was transferred to a 100 mL concentrated flask and the aqueous phase was added to 15 mL of ethyl acetate. The above procedure was repeated and the extracts were combined twice.
The evaporator was concentrated in a water bath at 40 ° C under reduced pressure to near dryness, dissolved in 8 mL of ethyl acetate and quantitatively transferred to a 10 mL centrifuge tube.
The following water bath with a gentle nitrogen flow to dry, accurately add 1 mL of ethyl acetate, mix, gas chromatographic determination.
7.2 Determination
7.3.1 Gas Chromatographic Reference Conditions
A) Column. quartz capillary column, DB-1701, 30 mx 0.25 mm (inner diameter) x 0.25 m (film thickness), or equivalent;
B) Carrier gas. nitrogen (purity greater than 99.999%); carrier gas flow rate 1.0 mL/min; tail gas flow rate. 30 mL/min; hydrogen flow rate.
75 mL/min, air flow rate. 100 mL/min;
C) Column temperature. initial temperature 50 ° C for 2 min, rise to 180 ° C at 15 ° C/min for 1 min, rise to 290 ° C at 8 ° C/min
Keep for 10 min;
D) Inlet temperature. 250 ° C;
E) Detector temperature. 250 ° C;
F) Injection method. no split injection;
G) Injection volume. 2 μL;
H) Opening time. 1.5 min.
7.3.2 Chromatographic determination
According to the content of organophosphorus pesticides in the sample, the standard working solution with similar peak area is selected. Standard working solution and sample solution
The response value of organophosphorus should be within the linear range of the instrument. Standard working solution and sample volume and other volume interspersed injection determination. In the above chromatographic conditions
The retention time of trichlorfon was about 6.0 min, the retention time of flocculent phosphorus was about 17.8 min, the retention time of chlorpyrifos was about 18.5 min,
The retention time of malathion was about 18.9 min, and the retention time of flocculent phosphorus was about 27.8 min. The chromatogram of the standard is shown in Appendix A.
Figure A.1.
7.4 blank experiment
In addition to the sample, according to the above determination steps.
8 results are calculated and expressed
Use the chromatographic data processor or calculate the organic phosphorus pesticide content in the sample according to the following formula (1).
MΑsi
VCsiAi
X
.. (1)
Where.
Xi - Residual content of each organophosphorus pesticide in the sample in milligrams per kilogram, mg/kg;
The peak area of each organophosphorus pesticide in the sample solution;
V - the final volume of the sample solution, in milliliters, mL;
Asi - the peak area of each organophosphorus pesticide in standard working fluid;
Csi - the concentration of organophosphorus pesticide in standard working fluid in micrograms per milliliter, g/mL;
M - the amount of 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 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 organic phosphorus pesticides is 0.01 mg/kg.
10.2 Recovery rate
The recoveries of the experimental data (in the range of different additive concentrations) are as follows.
A) trichlorfon.
1) the concentration of 0.01 mg/kg in the recovery rate of 70-85%, precision 6.0%;
2) The concentration of 0.02 mg/kg was 70-90% and the precision was 9.2%.
3) The recovery of 0.1 mg/kg was 81-89% and the precision was 3.2%.
B) Flies phosphorus.
1) the concentration of 0.01 mg/kg in the recovery rate of 73-99%, the precision of 10.0%;
2) The concentration of 0.02 mg/kg was 75-95% and the precision was 7.7%.
3) the recovery of 0.1 mg/kg in the recovery rate of 80-97%, precision 6.4%;
C) chlorpyrifos.
1) the concentration of 0.01 mg/kg in the recovery rate of 84-102%, precision 6.3%;
2) the concentration of 0.02 mg/kg in the recovery rate of 80-100%, the precision of 6.7%;
3) The concentration of 0.1 mg/kg was 84-106% and the precision was 8.5%.
D) malathion
1) added at the concentration of 0.01 mg/kg recovery rate of 84-106%, precision of 7.6%;
2) The concentration of 0.02 mg/kg was 80-105% and the precision was 10.0%.
3) The recovery rate was 81-103% and the precision was 7.6% at 0.1 mg/kg.
E) flies poison phosphorus
1) the concentration of 0.01 mg/kg in the recovery rate of 74-96%, the precision of 10.0%;
2) The concentration of 0.02 mg/kg was 75-100% and the precision was 10.4%.
3) The concentration of 0.1 mg/kg was 80-102% and the precision was 7.9%.
Appendix A
(Informative)
Standard chromatogram
Figure A.1 Gas chromatograms of five organophosphorus standards
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
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
Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 23200.97-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.97-2016_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time. Question 2: Can I share the purchased PDF of GB 23200.97-2016_English with my colleagues?Answer: Yes. The purchased PDF of GB 23200.97-2016_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet. Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to [email protected]. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay.
|