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GB 23200.29-2016: Food safety national standard -- Determination of residual residues of oxazabs in fruits and vegetables by liquid chromatography
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Food safety national standard -- Determination of residual residues of oxazabs in fruits and vegetables by liquid chromatography
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GB 23200.29-2016
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Basic data | Standard ID | GB 23200.29-2016 (GB23200.29-2016) | | Description (Translated English) | Food safety national standard -- Determination of residual residues of oxazabs in fruits and vegetables by liquid chromatography | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 8,868 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 1977-2007 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.29-2016: Food safety national standard -- Determination of residual residues of oxazabs in fruits and vegetables by liquid chromatography
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Food safety national standard - Determination of residual residues of oxazabs in fruits and vegetables by liquid chromatography
National Standards of People's Republic of China
GB
Instead of SN/T 1977-2007
National standards for food safety
Determination of the Residual Amount of Tetrazolium in Fruits and Vegetables
Liquid chromatography
National food safety standards-
Determination of fenpyroximate residue in fruits and vegetables
Liquid 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 1977-2007 "High Performance Liquid Chromatography for the Detection of the Residual Potatoes in Fruit and Vegetables."
Compared with SN/T 1977-2007, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the name "export fruit and vegetables" to "fruit and vegetables";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 1977-2007.
National standards for food safety
Determination of residual residues of oxazabs in fruits and vegetables by liquid chromatography
1 Scope
This standard specifies the method of high performance liquid chromatography for the determination of the residues of oxazolid in fruits and vegetables.
This standard applies to the citrus, cabbage, the determination of the residual amount of squalidomide; 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 methanol, n-hexane stripping, neutral alumina column, and detected by high performance liquid chromatography with UV detector.
Quantitative 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 Methanol (CH3OH). Chromatographic Purification.
4.1.2 n-hexane (C6H14). pure chromatography.
4.1.3 Ethyl acetate (C4H8O2). Chromatographic purity.
4.1.4 anhydrous sodium sulfate (Na2SO4). 650
C burning 4 h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve.
4.2 solution preparation
4.2.1 sodium chloride solution (10%). take 10 g of sodium chloride, the volume of water to 100 mL, shake back.
4.3 standards
4.3.1 Streptomide standard (Fenpyroximate, CAS.NO .. 111812-58-9). purity ≥99%.
4.4 standard solution preparation
4.4.1 Streptomide standard stock solution. accurately weighed appropriate amount of azole mite ester standard, with acetonitrile prepared into a concentration of 100 μg/mL standard reserve
liquid. According to the need to use acetonitrile diluted to the appropriate concentration of standard working fluid.
4.5 Materials
4.5.1 Neutral alumina solid phase extraction column. 1 000 mg, 3 mL.
5 instruments and equipment
5.1 High Performance Liquid Chromatograph with UV Detector.
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 Homogenizer. 5000 r/min.
5.4 Centrifuge. 4000 r/min.
5.5 Rotary Evaporator.
5.6 nitrogen blowing instrument.
5.7 Scroll Mixer.
6 Preparation and storage of samples
6.1 Preparation of the sample
To replace the sample of about 500 g, the sampling site according to GB 2763 Appendix A, the individual large samples need to be chopped, into the high-speed organization
The crusher is mashed evenly, packed in a clean container, sealed and marked with a mark.
6.2 Sample storage
Samples were stored at 0 - 4 ° C. 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 measurement steps
7.1 Extraction
Weigh 15 g (accurate to 0.01 g) sample placed in 50 mL centrifuge tube, add 20 mL of methanol, high-speed homogenization 2 min. 4000 r/min
Centrifuge 4 min, filter, add 20 mL of methanol residue, vortex 1 min, repeat centrifugal filtration operation, combined filtrate, to be purified.
7.2 Purification
The filtrate was transferred to a 250 mL separatory funnel, 40 mL of sodium chloride solution and 20 mL of n-hexane were added, vigorously shaken for 2 min,
The layers were placed in a 100 mL stoppered flask. The aqueous layer was repeatedly extracted with 20 mL of n-hexane and the n-hexane layer was combined.
Add 2 g of anhydrous sodium sulfate, shake, after standing, the n-hexane layer into the 100 mL concentrated bottle, and then a small amount of n-hexane washing with a plug cone
The bottles are washed twice and the washings are combined to the vials. In 40 ° C water bath rotation concentrated to near dry.
The flask was washed with 3 x 3 mL of n-hexane-ethyl acetate (28) and the solution was transferred to 5 mL of ethyl acetate pre-leached neutral oxygen
In the aluminum solid phase extraction column, the flow rate was controlled by about 2 mL/min, and the whole effluent was collected. Dried in a nitrogen bath at 40 ° C and dissolved in the mobile phase
Constant volume to 1.0 mL, over 0.45 μm filter for liquid chromatography analysis.
7.3 Determination
7.3.1 High Performance Liquid Chromatography Reference Conditions
A) Column. ZORBAX SB-C18,5 μm, 250 mm × 4.6 mm (id) or equivalent;
B) Mobile phase. acetonitrile - water (85 15).
C) Flow rate. 0.8 mL/min.
D) Detection wavelength. 254 nm.
E) Injection volume. 40 μL.
7.3.2 Determination and confirmation of chromatography
According to the test solution of azole mite content of the situation, selected peak area similar to the standard working solution. Standard working solution and sample solution of oxazolamate
The response value should be within the linear range of the instrument detection. Standard working solution and sample volume and other volume interspersed injection determination. Under the above chromatographic conditions,
The reference retention time of the azole was 9.8 min. The liquid chromatogram of the standard solution of the azole compound is shown in Figure A.1 in Appendix A.
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 processing software or the formula (1) to calculate the residual content of the azole in the sample.
A · c · V
X = ------ (1)
AS · m
Where.
X - the residual amount of oxazolidate in milligrams per kilogram, mg/kg;
A - the peak area of the solution of the ester solution;
AS - the peak area of the azole in the standard working fluid;
C - the standard working solution of the concentration of azole mites in micrograms per milliliter, μg/mL;
V - the final volume of the sample solution, in milliliters, mL;
M - the final sample of the sample quality, in grams, g.
Note. The result of the calculation is deducted from the blank value. The result of the measurement is expressed by the arithmetic mean of the parallel measurement, and the two valid digits are retained.
9 precision
9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the
Record 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 the
Record C requirements.
10% limit and recovery rate
10.1 Quantitation limits
The limit of this method is 0.02 mg/kg.
10.2 Recovery rate
10.2.1 Additive concentration and recovery of azoxystrobin in citrus experimental data.
The recoveries were 80.4% ~ 97.5% at the concentration of 0.02 mg/kg.
The recoveries were 83.5% ~ 97.1% at the concentration of 0.05 mg/kg.
When the concentration of azole was increased at 0.20 mg/kg, the recovery was 87.8% ~ 101.7%.
10.2.2 Chinese cabbage mites added concentration and recovery of experimental data.
The recoveries were 78.2% ~ 96.0% at the concentration of 0.02 mg/kg.
The recoveries were 81.7% ~ 97.4% at the concentration of 0.05 mg/kg.
The recoveries were 87.3% ~ 102.5% at the concentration of 0.20 mg/kg.
Appendix A
(Informative)
Standard chromatogram
Figure A.1 Schematic diagram of azolecarboxide standard liquid chromatography
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
> 1 19
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