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GB 23200.19-2016: Food safety national standard -- Determination of abamectin residues in fruits and vegetables -- Liquid chromatographic method
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Food safety national standard -- Determination of abamectin residues in fruits and vegetables -- Liquid chromatographic method
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GB 23200.19-2016
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Basic data | Standard ID | GB 23200.19-2016 (GB23200.19-2016) | | Description (Translated English) | Food safety national standard -- Determination of abamectin residues in fruits and vegetables -- Liquid 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Count Estimation | 9,936 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 2114-2008 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.19-2016: Food safety national standard -- Determination of abamectin residues in fruits and vegetables -- Liquid chromatographic method
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Food safety national standard - Determination of abamectin residues in fruits and vegetables - Liquid chromatographic method
National Standards of People's Republic of China
Instead of SN/T 2114-2008
National standards for food safety
Determination of abamectin residues in fruits and vegetables
Liquid chromatography
National food safety standards-
Determination of abamectin residue in fruits and vegetables
Liquid chromatography
2016-12-18 Release.2017-06-18 Implementation
Foreword
This standard replaces SN/T 2114-2008 "Determination of abamectin residues in fruits, vegetables and vegetables by liquid chromatography".
Compared with SN/T 2114-2008, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the name of the "import and export of fruits 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 2114-2008.
National standards for food safety
Determination of abamectin residues in fruits and vegetables - Liquid chromatographic method
1 Scope
This standard specifies the production of avermectins in fruits and vegetables and the method of liquid chromatography.
This standard applies to the detection of abamectin residues in apples and spinach. 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 method summary
The avermectin in the sample was extracted with acetone, concentrated, purified with SPE C18 column and eluted with methanol. The eluate was concentrated,
Constant volume, filtered, with a UV detector with high performance liquid 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 Acetone (C3H6O). Chromatographic pure.
4.1.2 Methanol (CH4O). Chromatographic purity.
4.2 standards
4.2.1 Avermectin standard (molecular formula C48H72O14). purity ≥ 96.0%.
4.3 standard solution preparation
4.3.1 Avermectin standard stock solution. Weigh 0.1 g (accurate to 0.0002 g) Avermectin standard in 100mL volumetric flask, with a
The alcohol was dissolved and set to a standard stock at a concentration of 1.0 mg/mL.
4.3.2 abamectin standard working solution. according to the need to remove the appropriate amount of avermectin standard stock solution, diluted with methanol to the appropriate concentration of the standard
quasi. Standard working fluid should be prepared once a week.
5 instruments and equipment
5.1 High Performance Liquid Chromatography. equipped with UV detector
5.2 Analysis of balance. 0.01 g and 0.0001 g
5.3 Tissue crusher.
5.4 Oscillator.
5.5 Rotary evaporator.
5.6 Solid phase extraction column. SPE C18. Specifications. 60 mg/3 mL Activated with 5 mL of methanol and 5 mL of water before use.
6 Preparation and storage of samples
6.1 Preparation of the sample
The sample was sorted out 1 kg, the sampling site according to GB 2763 Appendix A implementation, the sample was broken by the organization crusher, are divided into two,
Into a clean container, sealed as a sample and marked with a mark.
6.2 Sample storage
Store the sample below -18 ° C.
During sample and sample preparation, the sample should be protected from contamination or changes in the residue content.
7 Analysis steps
7.1 Extraction
Weigh the sample about 20 g (accurate to 0.1 g) in a 100 mL stoppered conical flask, add 50 mL of acetone, shake on an oscillator at 0.5
H Filtration with a Buchner funnel, washing the conical flask and residue with 20 mL x 2 acetone. The acetone extract was combined and evaporated to about 40 ° C in a water bath
2 mL.
7.2 Purification
The concentrated extract was transferred to the SPE C18 column and rinsed with 5 mL of water to remove the eluent. Finally eluted with 5 mL of methanol,
The eluate was collected and purged with nitrogen. Accurately add 1.0 mL of methanol to dissolve the residue, filter with 0.45 μm filter, the filtrate for the liquid phase
Chromatography. External standard method.
7.3 Determination
7.3.1 High Performance Liquid Chromatography Reference Conditions.
A) Column. ODS-C18 reverse phase column, 4.6 mm × 125 mm;
B) mobile phase. methanol. water = (90 10, V/V);
C) Flow rate. 1.0 mL/min;
D) Detection wavelength. 245 nm;
E) Column temperature. 40 ° C;
F) Injection volume. 20 μL.
7.3.2 Chromatographic determination
According to the content of avermectin in the sample solution, the standard working fluid in the standard working fluid and the concentration of avermectin in the sample solution
Should be in the instrument within the linear range of testing, the standard working fluid and sample volume and other volume injection. In the above chromatographic conditions, abamectin retention time
About 5.3 min.
For standard chromatograms, see Appendix A, Standard UV Spectra See Appendix B.
7.4 blank test
Except for the addition of samples, are carried out according to the above measurement steps.
8 results are calculated and expressed
Use the chromatographic data processor, or according to formula (1) to calculate the amount of abamectin residues in the sample.
X = h · c · V/hs · m (1)
Where.
X - the amount of abamectin residues in milligrams per kilogram (mg/kg);
H - the height of avermectin in the sample solution, in millimeters (mm);
Hs --- standard working solution of avermectin peak height, the unit is millimeter (mm);
C - standard concentration of avermectin in working fluid, in milligrams per liter (mg/L);
V - the final volume of the sample solution in milliliters (mL);
M --- the amount of sample that the final sample represents, 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 reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the
Record 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 the
Record the requirements of D.
10% limit and recovery rate
10.1 Quantitation limits
The quantification limit of this method is 0.01 mg/kg.
10.2 Recovery rate
Experimental data on the concentration and recovery of avermectin in apple samples.
The recovery was 82.5% at 0.01 mg/kg.
The recovery was 87.5% at 0.05 mg/kg.
The recovery was 95.0% at 0.50 mg/kg.
The experimental data on the concentration and recovery of avermectin in spinach.
The recovery was 83.0% at 0.01 mg/kg.
The recovery rate was 89.0% at 0.05 mg/kg.
The recoveries were 97.0% at 0.50 mg/kg.
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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