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GB 23200.17-2016: Food safety national standard -- Determination of Thiabendazole Residues in Fruits and Vegetables by Liquid Chromatography
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Food safety national standard -- Determination of Thiabendazole Residues in Fruits and Vegetables by Liquid Chromatography
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GB 23200.17-2016
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Basic data | Standard ID | GB 23200.17-2016 (GB23200.17-2016) | | Description (Translated English) | Food safety national standard -- Determination of Thiabendazole Residues in Fruits and Vegetables by Liquid Chromatography | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 10,113 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | NY/T 1649-2008 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.17-2016: Food safety national standard -- Determination of Thiabendazole Residues in Fruits and Vegetables by Liquid Chromatography
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Food safety national standard - Determination of Thiabendazole Residues in Fruits and Vegetables by Liquid Chromatography
GB
National Standards of People's Republic of China
Instead of NY/T 1649-2008
National standards for food safety
Determination of Thiabendazole Residues in Fruits and Vegetables
Liquid chromatography
National food safety standards-
Determination of thiabendazole 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 NY/T 1649-2008 "Determination of thiabendazole residues in fruits and vegetables by high performance liquid chromatography".
This standard and NY/T 1649-2008 compared to the main changes are as follows.
- the standard name has been modified to increase the national standard for food safety;
- modified in accordance with the format of the food safety standard.
- normative reference documents to increase the GB 2763 "maximum pesticide residues in food" standard;
- the preparation of the sample to increase the sampling site requirements and refine the requirements of the preparation of the sample;
- Increased precision requirements.
National standards for food safety
Determination of Thiabendazole Residues in Fruits and Vegetables by Liquid Chromatography
1 Scope
This standard specifies the method for the determination of thiabendazole residues in vegetables and fruits by high performance liquid chromatography (HPLC).
This standard applies to the determination of thiabendazole residues in vegetables and fruits.
2 normative reference documents
The following documents are indispensable for the application of this document. For dated filing applications, only the dated edition applies to this document.
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
Samples of thiabendazole in the sample after extraction, according to thiophanate in acidic conditions dissolved in water, alkaline conditions dissolved in the principle of ethyl acetate,
Purification, and then by the reverse phase chromatography, UV detector 300nm detection, according to the retention time qualitative, external standard method quantitative.
4 Reagents and Materials
Unless otherwise stated, only reagents identified as analytical reagents and water at GB/T 6682 level were used in the analysis.
4.1 Reagents
4.1.1 Methanol (CH3OH), chromatographic pure.
4.1.2 Ethyl acetate (CH3COOC2H5).
4.1.3 Sodium chloride (NaCl).
4.1.4 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, the dryer to save.
4.2 solution preparation
4.2.1 hydrochloric acid solution (0.1 mol/L). absorb 8.33 mL of hydrochloric acid, water volume to 1 L.
4.2.2 Sodium hydroxide solution (1.0 mol/L). Weigh 40 g of sodium hydroxide, dissolve in water and set to 1 L.
4.3 standards
Thiabendazole (CAS 148-79-8). purity greater than 99%.
4.4 standard solution preparation
Standard storage solution (100 mg/L). accurately weighed thymidazole 0.0100 g, dissolved in methanol, the volume to 100 mL, set 4 ℃ preservation,
Valid for 3 months.
5 instruments and equipment
5.1 High Performance Liquid Chromatograph with UV Detector.
5.2 Analysis of balance. 0.01 g and 0.1 mg.
5.3 Tissue crusher.
5.4 Rotary Evaporator.
5.5 Mechanical reciprocating oscillator.
5.6 Buchner funnel.
6 sample preparation
Sampling samples of vegetables and fruit samples according to GB 2763-2014 Appendix A sampling, for the smaller individual samples, after sampling the whole
For the individual large uniform sample can be split on the axis of symmetry or symmetry or cut into small pieces of post-processing; for slender, flat
Flat or component content in the various parts of the sample can be cut in different parts of small pieces or cut into small pieces or processing; take the sample after the chopped,
Fully mixed, with a quartile sampling or directly into the tissue crusher mashed into homogenate. The homogenate was placed in a polyethylene bottle at -16 ° C to -20 ° C
Save under the file.
7 Analysis steps
7.1 Extraction and purification
Weigh 10 g sample, accurate to 0.01 g, into a 250 mL stoppered flask, add 40 mL of methanol, homogenize 1 min,
Shaking on the shaker for 20 min, the Buchner funnel was filtered and the residue was washed twice with the appropriate amount of methanol. The filtrate was combined in a 150 mL pear flask.
50 ℃ under reduced pressure evaporated to the remaining 5 mL ~ 10mL, with 20 mL hydrochloric acid solution into the 250 mL separatory funnel, add 20 mL of ethyl acetate vibration
Swing, stand still, ethyl acetate layer and then 20 mL hydrochloric acid solution extraction time. The combined aqueous phase was adjusted to pH 8 to 9 with sodium hydroxide solution and 4 g was added
Sodium chloride, into the 250 mL separatory funnel, with 40 mL of ethyl acetate were extracted 2 times, combined with ethyl acetate, dehydrated by anhydrous sodium sulfate,
At 50 ° C under reduced pressure rotary evaporation near dry, the residue dissolved with mobile phase and volume to 5 mL, filtered through the 0.45μm filter to be tested.
7.2 Liquid Chromatographic Reference Conditions
Detector. UV detector.
Column. C18, 4.6 x 250 mm (5 μm) or equivalent.
W = (1)
B.
Mobile phase. methanol water = 50 50.
Flow rate. 1.0 mL/min.
Detection wavelength. 300 nm.
Column temperature. room temperature.
Injection volume. 10 μL.
7.3 Standard working curve
Absorb the standard stock solution 0 mL, 0.1 mL, 0.5 mL, 1 mL and 2 mL, with the mobile phase volume to 10 mL, this standard series of quality
The concentrations of 0 mg/L, 1.00 mg/L, 5.00 mg/L, 10.0 mg/L and 20.0 mg/L were used to determine the peak area as the ordinate and the corresponding standard
The mass concentration of the liquid is the abscissa, the standard curve is drawn, the regression equation and the correlation coefficient are obtained.
7.4 determination
The standard working solution and the test solution were injected into the high performance liquid chromatography, to retain the time qualitative, to be measured peak area into the standard
Quasi-curve in the quantitative, the sample concentration of thiabendazole concentration should be in the standard working curve mass concentration range. At the same time do blank test.
8 Results calculation.
The residual amount of thiabendazole in the sample is expressed in terms of mass fraction w, expressed in milligrams per kilogram (mg/kg), calculated according to formula (1)
× V
Where.
- The mass concentration of thiabendazole in the sample solution is calculated from the standard curve in milligrams per liter (mg/L);
V-final volume, in milliliters (mL);
M-sample mass in g (g).
The calculated results shall be deducted from the blank values and the calculated results shall be expressed as the arithmetic mean of the two independent determinations obtained under reproducible conditions.
Leave two valid digits.
9 precision
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 A requirements.
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 B requirements.
10% limit
The limit method of this standard method is 0.05mg/kg.
11 Chromatogram.
Thiabendazole standard solution map shown in Figure 1.
Figure 1 1.0mg/L thiabendazole standard solution map shown in Figure
Appendix A
(Normative appendix)
Laboratory repeatability requirements
Table A.1 Laboratory repeatability requirements
Measured component content
Mg/kg
Precision
0.001 36
> 0.01
> 1 14
Appendix B
(Normative appendix)
Inter-laboratory reproducibility requirements
Table B.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
Precision
0.001 54
> 0.01
> 1 19
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