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SN/T 2233-2020: (Determination of Fenpropathrin Residues in Exported Plant-derived Foods)
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(Determination of Fenpropathrin Residues in Exported Plant-derived Foods)
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SN/T 2233-2020
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| SN/T 2233-2008 | English | 799 |
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Determination of fenpropathrin residue in food for import and export
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SN/T 2233-2008
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PDF similar to SN/T 2233-2020
Basic data | Standard ID | SN/T 2233-2020 (SN/T2233-2020) | | Description (Translated English) | (Determination of Fenpropathrin Residues in Exported Plant-derived Foods) | | Sector / Industry | Commodity Inspection Standard (Recommended) | | Classification of Chinese Standard | C53 | | Classification of International Standard | 67.050 | | Word Count Estimation | 15,152 | | Date of Issue | 2020-12-30 | | Date of Implementation | 2021-07-01 | | Older Standard (superseded by this standard) | SN/T 2233-2008 | | Regulation (derived from) | General Administration of Customs Announcement No. 136 [2020] | | Issuing agency(ies) | General Administration of Customs | SN/T 2233-2020: (Determination of Fenpropathrin Residues in Exported Plant-derived Foods)---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.
Determination of fenpropathrin residue in plant original foods for export
The People's Republic of China Entry-Exit Inspection and Quarantine Industry Standards
Replace SN/T 2233-2008
Fenpropathrin in export plant-derived foods
Determination of residue
2020-12-30 release
2021-07-01 implementation
Issued by the General Administration of Customs of the People's Republic of China
Foreword
This document is compiled in accordance with the rules given in GB/T 1.1-2009.
This document replaces SN/T 2233-2008 "Methods for the Determination of Fenpropathrin Residues in Imported and Exported Foods", and is revised to be consistent with SN/T
Compared with 2233-2008, in addition to editorial changes, the main technical changes are as follows.
--Modified the file name;
--The scope of application of the document is extended to tomatoes, carrots, sweet peppers, red cabbage, spinach, leeks, celery, Chinese cabbage, eggplant, apples
Fruits, citrus, grapes, mushrooms, wheat, soybeans and tea.
--- Added gas chromatography tandem mass spectrometry as the first method in the document; the original standard gas chromatography as the second method;
- Modified the pre-processing method.
--The sampling step is omitted.
Please note that certain contents of this document may involve patents, and the issuing agency of this document does not bear the responsibility for identifying these patents.
This document was proposed and managed by the General Administration of Customs of the People's Republic of China.
This document was drafted by. Shanghai Customs of the People's Republic of China.
The main drafters of this document. Qu Li, Yang Huiqin, Zeng Jing, Li You, Deng Xiaojun, Zhu Jian.
The previous releases of this document are as follows.
Fenpropathrin in export plant-derived foods
Determination of residue
1 Scope
The first method of this document specifies the method for determination and confirmation of fenpropathrin residues in foods of plant origin for export by gas chromatography-tandem mass spectrometry.
The second law stipulates the gas chromatography-electron capture detector (ECD) method for the determination of fenpropathrin residues in exported plant-derived foods.
This document applies to tomatoes, carrots, sweet peppers, red cabbage, spinach, leeks, celery, Chinese cabbage, eggplant, apples, citrus,
Determination and confirmation of fenpropathrin residues in grapes, mushrooms, wheat, soybeans and tea.
2 Normative references
The contents of the following documents constitute the indispensable clauses of this document through normative references in the text. Among them, dated quotations
Only the version corresponding to that date is applicable to this document; for undated references, the latest version (including all amendments) is applicable
Used in this document.
GB/T 6682 Analytical laboratory water specifications and test methods
Method One Gas Chromatography Tandem Mass Spectrometry
3 Terms and definitions
There are no terms and definitions that need to be defined in this document.
4 Method summary
The residual fenpropathrin in the sample is extracted with acetonitrile or acetonitrile (containing 1% glacial acetic acid), and the dispersive solid phase extraction method is used for purification.
(EI) The gas chromatography-mass spectrometer/mass spectrometer of the ion source is used for quantification and confirmation detection, and the matrix standard solution external standard method is used for quantification.
5 Reagent materials
Unless otherwise specified, the reagents used are of analytical grade, and the water is the first grade water specified in GB/T 6682.
5.1 Acetonitrile. chromatographically pure.
5.2 n-Hexane. chromatographically pure.
5.3 Acetone. chromatographically pure.
5.4 Glacial acetic acid.
5.5 Anhydrous Magnesium Sulfate. Bake in a muffle furnace at 500°C for about 4 hours, and store in an airtight container for later use after cooling.
5.6 Sodium chloride.
5.7 Sodium citrate.
5.8 Disodium hydrogen citrate.
5.9 C18 adsorbent. 40 μm ~ 63 μm.
5.10 Graphitized carbon (Carbon-GCB) adsorbent. 120 mesh ~ 400 mesh.
5.11 Ethylenediamine-N-propylsilane (PSA) adsorbent. 40 μm ~ 60 μm.
5.12 Anhydrous sodium acetate. Bake in a muffle furnace at 500°C for about 4 hours, and store in a closed container for later use after cooling.
5.13 Acetonitrile (containing 1% acetic acid). Add 1 mL of acetic acid to 100 mL of acetonitrile, and mix well.
5.14 Fenpropathrin standard material (Fenpropathrin), the purity is greater than 95%. The Chinese and English name, CAS number, and minute of fenpropathrin
See the table A.1 in Appendix A for the sub-formula and other information.
5.15 Preparation of fenpropathrin standard stock solution. accurately weigh an appropriate amount of standard substance, dissolve it with acetonitrile and prepare it to a concentration of 1.0 mg/mL
Store the standard stock solution at -18°C in the dark.
5.16 Preparation of standard intermediate solution. Pipette 1.0 mL of the above standard stock solution into a 100 mL volumetric flask, dilute with acetonitrile and determine
Make it up to the mark, prepare a mixed standard intermediate solution of about 10μg/mL, and store at 0°C ~ 4°C in the dark.
5.17 Organic phase needle filter membrane. 0.22μm.
6 Apparatus and equipment
6.1 Gas chromatography-mass spectrometer/mass spectrometer. equipped with electron impact ionization source (EI).
6.2 Analytical balance. Sensitivity is 0.1mg and 0.01g respectively.
6.3 Vortex mixer.
6.4 Nitrogen blowing concentrator.
6.5 Centrifuge. the speed is not less than 4000r/min.
6.6 Grinder.
6.7 Organize the mixer.
6.8 Centrifuge tube with stopper. polypropylene, 15mL and 50mL.
7 Preparation and storage of samples
7.1 Vegetables and fruits
Take a representative sample of 500g, take the edible part and fully break it with a tissue mixer, mix it evenly, put it into a clean container, and seal it.
Indicate the mark.
7.2 Wheat and tea
Take a representative sample of 500g, smash all the samples with a grinder, and mix them; divide them into two samples and put them into clean containers.
Inside, sealed, marked with a mark.
7.3 Storage of samples
Vegetables and fruits are stored at -18°C; wheat and tea samples are stored below 4°C. During the sample preparation operation, the sample should be prevented from
Contaminated or changed in residue content.
8 Analysis steps
8.1 Extraction and purification
8.1.1 Vegetables and fruits
Weigh 10 g of a homogeneous sample (accurate to 0.01g) and place it in a 50 mL centrifuge tube (add 5.0 mL for dry vegetables
Water), add 10 mL acetonitrile (5.1), vortex for 2 min, add 4.0 g anhydrous magnesium sulfate (5.5), 1.0 g sodium chloride (5.6),
1.0 g sodium citrate (5.7) and 0.5 g disodium hydrogen citrate (5.8), shake vigorously for 10 min. Then centrifuge the tube at 4000 r/min
Heart for 5 minutes, transfer 8mL supernatant to a 15mL centrifuge tube, add.200 mg PSA (5.11),.200 mg C18 (5.9),
1000 mg anhydrous magnesium sulfate (5.5), vortex for 2 min, centrifuge at 4000 r/min for 5 min, take 5 mL of the supernatant and blow it to near dryness.
Vortex the residue with acetonitrile and dilute to 0.5 mL. It is filtered through a 0.22μm organic microporous filter membrane for determination by gas chromatography-mass spectrometry/mass spectrometer.
8.1.2 Cereals
Grain samples, crush and mix evenly, accurately weigh 2g (accurate to 0.01g), place it in a 50 mL centrifuge tube, and add 10.0 mL
After soaking in deionized water for 30 minutes, add 10 mL of acetonitrile solution (5.13) containing 1% acetic acid, vortex for 2 minutes, and add 4.0 g
Anhydrous magnesium sulfate (5.5), 1.0 g sodium chloride (5.6), 1.0 g sodium citrate (5.7) and 0.5 g disodium hydrogen citrate (5.8), shake vigorously
Swing for 10 minutes. Then the centrifuge tube was centrifuged at 4000 r/min for 5 min, and the 8 mL supernatant was transferred to a 15 mL centrifuge tube, and then added
Into 400 mg PSA (5.11), 400 mg GCB (5.10), 1200 mg anhydrous magnesium sulfate (5.5), vortex and mix for 2 min, 4000 r/min
Centrifuge for 5 min. Take 5 mL of the supernatant and blow it to near dryness. Vortex the residue with acetonitrile and dilute to 1.0 mL. Through 0.22 μm organic micropores
Membrane filtration for determination by gas chromatography-mass spectrometry/mass spectrometer.
8.1.3 Tea
Tea sample, crush and mix evenly, accurately weigh 2 g (accurate to 0.01g), place it in a 50 mL centrifuge tube, and add 10.0 mL
After soaking in deionized water for 30 minutes, add 10 mL of acetonitrile solution (5.13) containing 1% acetic acid, vortex for 2 minutes, and add 4.0 g
Anhydrous magnesium sulfate (5.5), anhydrous sodium acetate 1.0 g (5.12), shake vigorously for 10 min. Then the centrifuge tube was centrifuged at 4000 r/min for 5 min,
Transfer 8 mL of the supernatant to a 15 mL centrifuge tube, add 400 mg PSA (5.11), 400 mg GCB (5.10), 300 mg in turn
C18 (5.9), 1200 mg anhydrous magnesium sulfate (5.5), vortex for 2 min, centrifuge at 4000 r/min for 5 min, and take 5 mL of the supernatant
Blow nitrogen to near dryness, vortex the residue with acetonitrile and dilute to 1.0 mL. Filtered by 0.22 μm organic microporous filter membrane for gas chromatography-mass spectrometry/
Determination by mass spectrometer.
8.1.4 GC-MS/MS confirmation reference conditions
The GC-MS/MS instrument reference conditions are as follows.
a) Chromatographic column. DB-5MS capillary column, 30 m × 0.25 mm (inner diameter) × 0.25 μm (film thickness) or equivalent;
b) Column temperature. the initial temperature is 60 ℃, keep it for 1 min, raise the temperature to 280 ℃ at 30 ℃/min, keep it for 2 min, and then increase it at 120 ℃/min
Raise the temperature to 300 ℃ and keep it for 5 min;
c) Injection port. programmed temperature injection, the initial temperature is 70 ℃, hold for 0.1 min, and the temperature is increased to 280 ℃ at 360 ℃/min;
d) Gas chromatography-mass spectrometry/mass spectrometry interface temperature. 290 ℃;
e) Carrier gas. helium, with a purity greater than or equal to 99.999%; constant flow mode; flow rate. 1.0 mL/min;
f) Injection volume. 5.0 μL;
g) Sampling method. splitless sampling;
h) Ionization source. electron bombardment ion source (EI source);
i) Ionization energy. 70 eV;
j) Solvent delay time. 6.0 min;
k) Scan mode. Multi-reactive ion monitoring mode (MRM), see Table A.1 in Appendix A for details of ion pair conditions.
8.1.5 Qualitative determination
Under the same experimental conditions, the retention time of the substance to be tested in the sample differs from the corresponding retention time in the standard working solution.
Within ±2.5%; after subtracting the background, the mass spectra of the tested sample and the standard are similar, and all the selected monitoring ions are
When the abundance ratio is consistent, and the allowable deviation does not exceed the range specified in Table 1, it can be determined that the drug is present in the sample
Residue.
8.1.6 Quantitative determination
In order to reduce the influence of the matrix on the quantification of the results, this method uses a negative sample solution to prepare a matrix-matched standard working solution.
Method quantification, according to the measured fenpropathrin residue content in the sample solution, select a standard working solution with a similar peak area. Standard working fluid and
The response value of the analyte in the sample solution should be within the linear range of the instrument, and the standard working solution and sample solution should be measured according to the same volume.
Insert sample measurement. Refer to Figure B.1 in Appendix B for the multi-reaction monitoring chromatogram of fenpropathrin; refer to Appendix C for the total ion chromatogram of fenpropathrin
In Figure C.1.
8.2 Blank test
Except that no sample is added, all follow the above steps.
9 Calculation and expression of results
Calculate the content of the fenpropathrin compound in the sample with a chromatographic data processor or according to formula (1). The calculation result needs to deduct the blank value.
10 Low limit of determination, recovery rate
10.1 Lower limit of determination
Use this method to treat tomatoes, carrots, sweet peppers, red cabbage, spinach, leeks, celery, Chinese cabbage, eggplant, apples, citrus,
Fenpropathrin residues in 16 kinds of matrices including grapes, mushrooms, wheat, soybeans and tea were determined. Gas chromatography-tandem mass spectrometry was used to remove wheat,
The lower limit of determination of various substrates other than soybean tea is 0.005 mg/kg, the lower limit of determination of wheat and soybean is 0.01 mg/kg, and the lower limit of determination of tea is 0.005 mg/kg.
It is 0.05mg/kg.
10.2 Recovery rate
Use this method to treat tomatoes, carrots, sweet peppers, red cabbage, spinach, leeks, celery, Chinese cabbage, eggplant, apples, citrus,
16 kinds of substrates including grapes, mushrooms, wheat, soybeans and tea were added to the recovery rate test. The addition level and recovery of fenpropathrin...
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