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SN/T 0491-2019

Chinese Standard: 'SN/T 0491-2019'
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SN/T 0491-2019EnglishRFQ ASK Days<=3 (Method for detection of phenflusulfamine residues in foods of plant origin for export) Valid SN/T 0491-2019
SN/T 0491-2019ChineseRFQ ASK <=1-day [PDF from Chinese Authority, or Standard Committee, or Publishing House]  

   

BASIC DATA
Standard ID SN/T 0491-2019 (SN/T0491-2019)
Description (Translated English) (Method for detection of phenflusulfamine residues in foods of plant origin for export)
Sector / Industry Commodity Inspection Standard (Recommended)
Date of Issue 2019-10-25
Date of Implementation 2020-05-01
Older Standard (superseded by this standard) SN 0491-1995
Regulation (derived from) General Administration of Customs Announcement No. 166 of 2019
Issuing agency(ies) General Administration of Customs

SN/T 0491-2019
(Method for detection of phenflusulfamine residues in foods of plant origin for export)
ICS 67.050C53
People's Republic of China Entry-Exit Inspection and Quarantine Industry Standard
SN/T 0491-2019 replaces SN/T 0491-1995
Fensulfonamide in plant-derived food for export
Residue detection method
Published on October 19,.2015
2020-05-01 implementation
Published by the General Administration of Customs of the People's Republic of China
Foreword
This standard was prepared in accordance with the requirements of GB/T 1.1-2009.
This standard replaces SN 0491-1995 "Test Method for Bacteriphos Residues in Grains for Export" This standard is in line with SN 4901-1995
The main technical changes are as follows.
--- This standard adds rice, wheat, soybean, corn, pear, grape, tomato, cucumber, potato, mushroom, dried pepper test samples
Matrix
--- Added confirmation of gas chromatography-mass spectrometry;
--- deleted the sampling part;
--- Optimized the pre-processing method;
Please note that some elements of this document may involve patents. The issuer of this document is not responsible for identifying these patents.
This standard is proposed and managed by the General Administration of Customs of the People's Republic of China.
This standard was drafted. Shijiazhuang Customs, People's Republic of China
The main drafters of this standard. Li Wei, Wang Jing, Ai Lianfeng, Ma Yusong, Chen Ruichun, Guo Chunhai, Zhang Haichao
The previous versions of the standards replaced by this standard are.
--- SN 0491-1995.
SN/T 0491-2019
Fensulfonamide in plant-derived food for export
Residue detection method
1 Scope
This standard specifies the gas chromatographic detection method and gas chromatography-mass spectrometry confirmation method of benzylsulfonamide residues in foods of plant origin for export.
This standard applies to benzsulfonamide in rice, wheat, soybean, corn, brown rice, pear, grape, potato, tomato, cucumber, mushroom and dried pepper.
Determination of residual amount.
2 Normative references
The following documents are essential for the application of this document. For dated references, only the dated version applies to this document.
file. For undated references, the latest version (including all amendments) applies to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
3 Method summary
The analytes in the sample were extracted with acetonitrile. The extract was concentrated and purified by a silica gel solid-phase extraction column for gas chromatography and gas chromatography.
Confirmed by spectrum-mass spectrometry and quantified by external standard method.
4 reagents and materials
Unless otherwise specified, the reagents are of analytical grade and the water is the first-grade water specified in GB/T 6682.
4.1 Acetonitrile, pure by high performance liquid chromatography.
4.2 n-hexane, pure by high performance liquid chromatography.
4.3 Ether.
4.4 Acetone, pure by high performance liquid chromatography.
4.5 Anhydrous sodium sulfate. Bake at 650 ° C for 4h, cool to room temperature in a desiccator, and store in a sealed bottle for later use.
4.6 N-hexane-ether (3 + 47, V/V). Take 30mL of n-hexane (4.2) and 470mL of ether (4.3) and mix well.
4.7 N-hexane-ether (1 + 1, V/V). Take 100mL of n-hexane (4.2) and 100mL of ether (4.3) and mix well.
4.8 Standard product. phenylfluorosulfanil (dichlofluid, C9H11C12FN2O2S2, CASN O. 1085-98-9), with a purity of 99% or more.
4.9 Standard stock solution. Accurately weigh an appropriate amount of standard product (4.8), and prepare 1.0 mg/mL standard stock solution with acetone (4.4). Avoid at 4 ° C.
Light preservation, storage period is 1 year.
4.10 Standard intermediate working solution. Take standard stock solution (4.9) from 1,000mL to 100mL volumetric flask, make up to the mark with acetone (4.4), prepare
Prepare a standard intermediate working solution with a concentration of 10.0 μg/mL and store it at 4 ° C in the dark, with a shelf life of 3 months.
4.11 Standard working solution. Absorb an appropriate amount of standard intermediate solution (4.10) according to the needs of the experiment, and dilute with acetone (4.4) to a standard of appropriate concentration.
Quasi-working solution, ready to use.
4.12 Silica gel solid phase extraction column. 500mg, 6mL; or equivalent.
4.13 Microporous membrane. 0.22 μm, organic phase type.
SN/T 0491-2019
5 instruments and equipment
5.1 Gas chromatograph. Equipped with an electronic capture detector (ECD).
5.2 Gas tandem mass spectrometer. Equipped with electron impact ionization source (EI)
5.3 Organization of mashers.
5.4 Electronic balance. Sensitivity is 0.01g and 0.1mg respectively.
5.5 Centrifuge. The rotation speed is not less than 5000r/mm.
5.6 Homogenizer. The rotation speed is not less than 1500r/min.
5.7 Nitrogen blowing instrument.
5.8 Rotary evaporator.
5.9 Solid-phase extraction device.
5.10 Polypropylene centrifuge tubes. 50mL and 15mL, with stoppers.
5.11 10mL glass graduated test tube.
5.12 Chicken heart bottle. 120mL.
6 Sample preparation and storage
6.1 Sample preparation requirements
During sample preparation, the sample should be protected from contamination or changes in the content of residues.
6.2 Sample preparation
6.2.1 Pear, grape, potato, tomato, cucumber, mushroom and dried pepper
Take a representative sample of 500g, pear, tomato, cucumber and dried pepper to take the whole fruit and remove the handle; grapes to take the whole fruit. potatoes and mushrooms take the whole one, use a masher to process the sample into a slurry and mix. The samples were divided into two parts, put into clean containers, sealed and marked. Below -18 ℃
Cryopreserved.
6.2.2 Rice, corn, wheat, soybeans and brown rice
Take a representative sample of 500g, take the whole grain, crush it with a pulverizer, and mix. The samples were divided into two parts, put into clean containers, sealed and marked. Store at room temperature.
7 Measurement steps
7.1 Extraction
7.1.1 Pear, grape, potato, tomato, cucumber and mushroom
Weigh about 5g of the sample (accurate to 0.01g) into a 50mL centrifuge tube, add 10g of anhydrous sodium sulfate (4.5), 20mL of acetonitrile (4.1),
1500r/min was homogeneously extracted for 2min, 4,000r/min was centrifuged for 10min, and the supernatant was filtered through a funnel containing 10g of anhydrous sodium sulfate (4.5) into a 120mL chicken heart bottle. Repeat the above extraction process with 15mL of acetonitrile. Combine the extracts in the same chicken heart bottle at 45 ° C.
Concentrate the water bath to dryness and wait for purification.
7.1.2 Rice, corn, wheat, soybeans, brown rice and dried peppers
Weigh about 2g of dried pepper sample, about 5g (accurate to 0.01g) of rice, corn, wheat, soybean and brown rice sample in 50mL centrifuge tube
SN/T 0491-2019
Add 10mL of water to wet the sample, mix it for 2min, leave it for 30min and add 10g of anhydrous sodium sulfate (4.5), 20mL of acetonitrile (4.1),
1500r/min homogeneous extraction 2min, 4,000r/min centrifugation 10min, the supernatant was passed through a funnel containing 10g anhydrous sodium sulfate (4.5)
Strain into 120mL chicken heart bottle. Repeat the above extraction process with 15mL of acetonitrile. Combine the extracts in the same chicken heart bottle at 45 ° C.
Concentrate the water bath to dryness and wait for purification.
7.2 purification
Dissolve the concentrate obtained in step 7.1 with 5 mL of n-hexane (4.2). Pre-washed silica gel solid phase extraction with 5 mL of n-hexane (4.2)
Column (4.12), pass the sample extraction solution through the solid phase extraction column, rinse the solid phase extraction column with 6 mL of n-hexane-diethyl ether (4.6) solution, and discard all the flow
The effluent was eluted with 2 mL of n-hexane-diethyl ether (4.7) solution. The entire effluent was collected and dried at 45 ° C under nitrogen. With 2.0mL of n-hexane
(4.2) After dissolution, after passing through the 0.22 μm organic phase microporous membrane, it is provided for gas chromatography determination and gas chromatography-mass spectrometry confirmation.
7.3 Gas chromatography
7.3.1 Gas chromatography reference conditions
The gas chromatography conditions are as follows.
a) Chromatographic column. DB-1701 quartz capillary column, 30m × 0.25mm (i.d), 0.25μm, or equivalent;
b) Column column heating program. 80 ° C (2min) 30 ° C/→/min200 ° C 5 ° C/→ min250 ° C (3min);
c) inlet temperature. 250 ° C;
d) Detector temperature. 300 ° C;
e) Carrier gas. nitrogen, purity 99.99%, flow rate. constant current mode 3mL/min;
f) sampling method. no split;
g) Injection volume. 2.0 μL.
7.3.2 Determination by gas chromatography
Under the optimal working conditions of the instrument, gas chromatography was quantified by external standard method. Select the peak surface according to the content of the analyte in the sample solution
Accumulate similar standard working solutions. The response value of the test substance in the standard working solution and sample solution should be within the linear range of the instrument.
Beyond the linear range, dilute with n-hexane (4.2) to the appropriate concentration and analyze. The standard working solution and the sample solution are sampled at the same volume.
Under the above chromatographic conditions, the reference retention time of phenflusulfamine is about 12.07 min. The gas chromatogram is shown in Figure A of Appendix A. 1.
7.4 Confirmation by gas chromatography-mass spectrometry
7.4.1 GC-MS reference conditions
The GC-MS conditions are as follows.
a) Chromatographic column. DB-5MS (30m × 0.25mm × 0.25μm) quartz capillary column, or equivalent;
b) Column temperature program. Hold at 60 ° C for 2 min, then raise the temperature to 220 ° C with the 30 ° C/min program, and then raise the temperature at 5 ° C/min.
To 250 ℃, keep 5min;
c) inlet temperature. 250 ° C;
d) Chromatography-mass spectrometry interface temperature. 280 ° C;
e) Ion source temperature. 230 ° C;
f) Carrier gas. Helium, purity ≥99.99%, flow rate 1.0mL/min;
g) Sample injection method. splitless injection. After 1.0 min, open the split valve and septum purge valve;
h) Ionization method. electron impact source (EI);
i) Injection volume. 1 μL;
SN/T 0491-2019
j) Measurement method. Select ion monitoring method;
k) Selecting monitoring ions (m/z). 123, 167, 224, 332 (abundance ratio 100. 45. 30. 6).
l) Solvent delay. 6 min;
m) Ionization energy. 70 eV.
7.4.2 Confirmation by gas chromatography mass spectrometry
It is confirmed that the retention time of the chromatographic peak of the analyte is consistent with that of the standard sample, and the sample spectrum after the background subtraction is selected.
All ions appear; at the same time, the abundance ratio of the selected ions is consistent with the relative abundance of related ions in the standard sample, and the similarity is within the allowable deviation.
(See Table 1), then the sample can be determined to be positive for fenflusulfa. GC-MS selective ion chromatogram of phenylsulfonamide standard material and
The mass spectrum is shown in Figure A in Appendix A. 2 and A. 3.
Table 1 Maximum allowable error of relative ion abundance during qualitative confirmation
Relative ion abundance /% > 50 > 20 ~ 50 > 10 ~ 20 ≤10
Allowable relative error /% ± 10 ± 15 ± 20 ± 50
7.5 Blank test
Except that no sample is added, the sample blank experiment is performed according to the above measurement conditions and procedures.
8 Calculation and presentation of results
Gas chromatographic method was used to determine the residual amount of phenylflusulamide in the sample using the standard curve method. The quantitative result of the standard curve method was calculated according to formula (1).
Calculation results need to deduct blank values.
In the formula.
Note. The calculation result should be deducted from the blank value.
9 Limit of quantitation and recovery
9.1 Limit of quantitation
The limit of quantification of this standard for rice, corn, wheat, soybeans, brown rice, pears, grapes, potatoes, cucumbers, tomatoes and mushrooms is 0.01 mg/kg; dry
The limit of quantification of pepper is 0.05 mg/kg.
9.2 Recovery rate
See Table B in Appendix B for the recovery range of different substrates and different addition levels. 1.
SN/T 0491-2019
Appendix A
(Informative appendix)
Chromatogram of Phenylfluorosulfone Standard
SN/T 0491-2019
SN/T 0491-2019
Appendix B
(Informative appendix)
Recovery rate
Table B. 1 The concentration and recovery data of the sample
Additive amount of matrix (mg/kg)
Recovery range
(%) Substrate
Added amount
(Mg/kg)
Recovery range
(%)
Rice
0.01 76.0-100.5
0.02 78.0-100.5
0.1 84.2-1000.4
brown rice
0.01 79.0-99.0.0
0.02 77.5-100.3
0.1 84.9-103.4
wheat
0.01 77.0-103.0
0.02 78.0-100.5
0.1 81.8-105.4
potato
0.01 79.0-100.3
0.02 80.0.5-100.5
0.1 86.9-102.2
corn
0.01 75.0-100.3
0.02 78.2-101.0.0
0.1 82.9-102.1
5 83.8-101.4
0.01 84.0-100.5
0.02 84.0-100.8
0.1 87.5-102.1
5 86.6-100.2
Soy
0.01 75.0-104.0
0.02 74.0-98.5
0.1 81.5-102.1
0.2 84.0-106.0
grape
0.01 79.0-100.3
0.02 79.5-101.0
0.1 84.4-101.4
15 85.2-100.3
tomato
0.01 79.0-107.0
0.02 81.0-100.5
0.1 84.9-103.1
2 84.0-102.5
mushroom
0.01 76.0-100.8
0.02 79.0-106.0
0.1 81.2-102.1
5 83.8-100.2
cucumber
0.01 82.0-104.0
0.02 82.5-106.0
0.1 87.4-101.2
5 87.8-100.4
Dried chili
0.05 75.0-106.0
0.1 80.9-100.5
0.5 82.0-102.0
20 81.6-100.1
SN/T 0491-2019
P. R. C.
-SN 04491-1995.
SN/T 0491-2019
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0.01 76.0-100.5
0.02 78.0-100.5
0.1 84.2-1000.4
0.01 79.0-99.0.0
0.02 77.5-100.3
0.1 84.9-103.4
0.01 77.0-103.0
0.02 78.0-100.5
0.1 81.8-105.4
0.01 79.0-100.3
0.02 80.0.5-100.5
0.1 86.9-102.2
0.01 75.0-100.3
0.02 78.2-101.0.0
0.1 82.9-102.1
5 83.8-101.4
0.01 84.0-100.5
0.02 84.0-100.8
0.1 87.5-102.1
5 86.6-100.2
0.01 75.0-104.0
0.02 74.0-98.5
0.1 81.5-102.1
0.2 84.0-106.0
0.01 79.0-100.3
0.02 79.5-101.0
0.1 84.4-101.4
15 85.2-100.3
0.01 79.0-107.0
0.02 81.0-100.5
0.1 84.9-103.1
2 84.0-102.5
0.01 76.0-100.8
0.02 79.0-106.0
0.1 81.2-102.1
5 83.8-100.2
0.01 82.0-104.0
0.02 82.5-106.0
0.1 87.4-101.2
5 87.8-100.4
0.05 75.0-106.0
0.1 80.9-100.5
0.5 82.0-102.0
20 81.6-100.1
SN/T 0491-2019
Related standard:   SN/T 0800.10-2019  SN/T 0173-2018
   
 
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