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GB 23200.87-2016: Food safety national standard -- Determination of thiabendazole residues in milk and dairy products -- Fluorescence spectrophotometric method
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Food safety national standard -- Determination of thiabendazole residues in milk and dairy products -- Fluorescence spectrophotometric method
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GB 23200.87-2016
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Basic data | Standard ID | GB 23200.87-2016 (GB23200.87-2016) | | Description (Translated English) | Food safety national standard -- Determination of thiabendazole residues in milk and dairy products -- Fluorescence spectrophotometric method | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 10,176 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN 0606-1996 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.87-2016: Food safety national standard -- Determination of thiabendazole residues in milk and dairy products -- Fluorescence spectrophotometric method
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Food safety national standard - Determination of thiabendazole residues in milk and dairy products - Fluorescence spectrophotometric method
National Standards of People's Republic of China
GB
Instead of SN 0606-1996
National standards for food safety
Determination of thiabendazole residues in milk and dairy products
Fluorescence spectrophotometry
National food safety standard-
Determination of thiabendazole residue in milk and milk products
Fluorescence spectrophotometry
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 0606-1996 "Test method for the determination of thiabendazole residues in milk and dairy products by fluorescence spectrophotometry".
Compared with SN/T 0606-1996, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- "Milk and dairy products" in the standard name "Export milk and dairy products";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
SN/T 0606-1996.
National standards for food safety
Determination of thiabendazole residues in milk and dairy products - Fluorescence spectrophotometric method
1 Scope
This standard specifies sampling, sample preparation and fluorescence spectrophotometric methods for the determination of thiabendazole residues in milk and dairy products.
This standard applies to the detection of thiabendazole residues in fresh milk, 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 fats in the sample were saponified with potassium hydroxide, and the thiabendazole was extracted with ethyl acetate. The extract of ethyl acetate was extracted with hydrochloric acid solution
Determination of Fluorescence Spectrophotometry, Quantitative Determination of 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 Potassium hydroxide (KOH).
4.1.2 Hydrochloric acid (HCl).
4.1.3 Ethyl acetate (CH3COOH).
4.2 solution preparation
4.2.1 50% (m/V) potassium hydroxide solution. accurately weighed 50 g of potassium hydroxide solid, dissolved in water, cooled to 100 mL,
Shaking back.
4.2.2 0.05% (m/V) potassium hydroxide solution. accurate removal of 50% potassium hydroxide solution (4.2.1) 1mL in 1000 mL volumetric flask,
Water volume, shake back spare.
4.2.3 0.1 mol/L hydrochloric acid solution. accurate removal of 0.83 mL concentrated hydrochloric acid in a 100 mL volumetric flask, the volume of water, shake back.
4.3 standards
4.3.1 Thiabendazole standard. purity ≥ 99%.
4.4 standard solution preparation
4.4.1 Thiabendazole standard stock solution. accurately weighed the appropriate amount of thiabendazole standard, with hydrochloric acid solution dubbed the concentration of 0.100 mg/mL
Standard stock solution. According to the need to use hydrochloric acid solution diluted to the appropriate concentration of standard working solution. Store in 4 ℃ refrigerator.
5 instruments and equipment
5.1 fluorescence spectrophotometer.
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 Condensate tube.
5.4 Separate funnel. 125 mL.
5.5 Erlenmeyer flask. 100 mL, with a grinding mouth.
5.6 electric hot water bath.
5.7 volumetric flask. 10 mL, 100 mL, 1000 mL.
6 Preparation and storage of samples
6.1 Preparation of the sample
The retrieved vials were thoroughly mixed and about 250 mL was taken as a sample. Into a clean container, sealed, marked mark.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
6.2 Sample storage
Store the sample below -5 ° C.
Note. During sampling and sample preparation, it is necessary to prevent contamination of the sample or change in the content of the residue.
7 Analysis steps
7.1 Saponification
Weigh the sample 10 g (accurate to 0.1 g) in the conical flask, add 7 mL of potassium hydroxide solution, connected to the condenser, in the boiling water bath
Reflux saponification 40 min, remove, fully cooled.
7.2 Extraction
The saponified solution was transferred to a separatory funnel and the Erlenmeyer flask was washed with 10 mL of water and the lotion was incorporated into the same separatory funnel. Add 15 mL of ethyl acetate
Ester, gently shake 0.5 min, static stratification. The aqueous layer was transferred to another separatory funnel, extracted again with 15 mL of ethyl acetate, shaken vigorously for 1 min,
Static stratification. The ethyl acetate extracts were combined.
7.3 purification
The ethyl acetate extract was washed with 20 mL of potassium hydroxide solution, shaken vigorously for 1 min, and the layers were discarded and the aqueous layer was discarded. Add another 20 mL
The potassium hydroxide solution was washed gently and the water was discarded. The ethyl acetate layer was extracted with 2 x 5 mL hydrochloric acid solution. The combined hydrochloric acid extract was added at 10 mL
Volumetric flask, and with hydrochloric acid solution volume. Determination by fluorescence spectrophotometry.
7.4 determination
7.4.1 Fluorescence spectrophotometric determination of the reference conditions
Excitation wavelength. 307 nm; emission wavelength. 359 nm. Different models of equipment, according to the actual situation to adjust to get the best excitation wave
Long and emission wavelengths.
7.4.2 Drawing of standard curves
Respectively, draw 0.2, 0.5, 1.0, 5.0 and 10.0 mL standard stock solution to a group of 10 mL volumetric flask, with hydrochloric acid solution volume,
The fluorescence absorbance was measured on a fluorescence spectrophotometer and the standard curve was plotted against the concentration of thiabendazole by fluorescence absorbance. The fluorescence of the standard light
The scan of the scale is shown in Figure A1 in Appendix A.
7.4.3 Determination of sample solution
The fluorescence intensity of the sample solution was measured on a fluorescence spectrophotometer. From the standard curve on the sample solution of thiophene
Bacteria concentration.
7.5 blank experiment
In addition to the sample, according to the above determination steps.
8 results are calculated and expressed
Calculate the residual content of thiabendazole in the sample according to formula (1)
Vc
.. (1)
Where. X-sample thiabendazole content, mg/kg;
C - the concentration of thiabendazole in the sample solution from the standard curve, μg/mL;
V - volume of sample solution after volume, mL;
M - the weight of the sample, g.
Note. The result of the calculation must be deducted from the blank value. The result of the measurement is expressed as 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 reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix C 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 D requirements.
10% limit and recovery rate
10.1 Quantitation limits
The limit of this method is 0.02 mg/kg.
10.2 Recovery rate
The recovery of thiabendazole is given in Appendix B.
Appendix A
Standard Fluorescence Absorbance Scanning Chart
Figure A1 Thiabendazole standard Fluorescence absorbance scan
Appendix B
(Informative)
Thiabendazole added levels and added recovery rates
Table B.1 Thiabendazole added levels and added recovery rates
Add level
(Mg/kg)
Recovery rate
(%)
0.02 102
0.10 96.5
0.50 99.6
Appendix C
(Normative appendix)
Laboratory repeatability requirements
Table C.1 Laboratory repeatability requirements
Measured component content
Mg/kg
Precision
0.001 36
> 0.01
> 1 14
Appendix D
(Normative appendix)
Inter-laboratory reproducibility requirements
Table D.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
Precision
0.001 54
> 0.01
> 1 19
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