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SN/T 1017.6-2019

Chinese Standard: 'SN/T 1017.6-2019'
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SN/T 1017.6-2019EnglishRFQ ASK Days<=3 Method for the determination of tecloftalam residues in cereals for export Valid SN/T 1017.6-2019
SN/T 1017.6-2019ChineseRFQ ASK <=1-day [PDF from Chinese Authority, or Standard Committee, or Publishing House]  

   

BASIC DATA
Standard ID SN/T 1017.6-2019 (SN/T1017.6-2019)
Description (Translated English) Method for the determination of tecloftalam residues in cereals 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Older Standard (superseded by this standard) SN/T 1017.6-2002
Regulation (derived from) General Administration of Customs Announcement No. 166 of 2019
Issuing agency(ies) General Administration of Customs

SN/T 1017.6-2019
(Detection method of cumene residue in grains for export)
ICS 67.050C53
People's Republic of China Entry-Exit Inspection and Quarantine Industry Standard
SN/T 1017.6-2019 instead of Sn/T 1017.6-2002
Detection method of cumene residue in grains for export
Published on October 19,.2015
2020-05-01 implementation
Published by the General Administration of Customs of the People's Republic of China
Foreword
SN/T 1017 is divided into the following nine parts.
--- Part 1. Inspection method of cycloheptafen residue in export grain;
--- Part 2. Inspection method for methamphetamine residues in exported grain;
--- Part 3. Test methods for pentosalone residues in exported grains and vegetables;
--- Part 4. Inspection method for pyridzolium residues in oilseeds for export;
--- Part 5. Inspection method for fast-killing radon residue in oilseeds for export;
--- Part 6. Test method for cumene residue in exported grain;
--- Part 7. Determination of Aldicarb, Menadicarb, Xantharcarb, Epicarb, and Aphicarb in Export Grains;
--- Part 8. Test methods for imidacloprid residues in imported and exported grains by liquid chromatography;
--- Part 9. Inspection method for piracetin residues in imported and exported grains.
This section is Part 6 of the Sn/T 1017.
This section is prepared in accordance with the rules given in GB/T 1.1-2009.
This section replaces SN/T 107.6-2002 "Examination Methods for Cucumin Residues in Grains for Export".
Compared with Sn/T 107.6-2002, the main technical changes in this section are as follows.
--- Added liquid chromatography-tandem mass spectrometry as the first method;
--- The original method was changed to the second method, and some expressions were modified;
--- Deleted the sampling step.
This section is proposed and managed by the General Administration of Customs of the People's Republic of China.
This section was drafted. Tianjin Customs, People's Republic of China.
The main drafters of this section. Zhang Yi, Lou Tingting, Cui Ying, Lin Anqing, Zhang Liangwen.
The previous versions of the standards replaced by this section are.
--- SN/T 1017.6-2002.
SN/T 1017.6-2019
Detection method of cumene residue in grains for export
1 Scope
This section specifies the gas chromatography and liquid chromatography-tandem mass spectrometry methods for determination of cumene residues in grains.
The first method in this part applies to the quantitative determination and confirmation of cumene residues in brown rice, wheat, corn, and lentils for export;
The second method in this part is applicable to the quantitative determination of cumene residue in brown rice for export.
2 Normative references
The following documents are essential for the application of this document. For dated references, only the dated version applies to this article
Pieces. For undated references, the latest version (including all amendments) applies to this document.
GB/T 6682 Analytical laboratory water specifications and test methods
First method liquid chromatography-mass spectrometry/mass spectrometry
3 Method summary
The sample was immersed in water, and cumene was extracted with methanol, and purified by solid phase extraction. It was detected by liquid chromatography-mass spectrometry/mass spectrometry and quantified by external standard method.
4 reagents and materials
Unless otherwise specified, the reagents used are of analytical grade, and the water is first-grade water specified in GB/T 6682.
4.1 Methanol. chromatographically pure.
4.2 Formic acid. chromatographically pure.
4.3 Formic acid aqueous solution (0.1%). Absorb 1mL of formic acid, make up to 1L with water, and mix well.
4.4 Diatomaceous earth.
4.5 Luteumphthalein standard substance (Teflocalam, CAS No. 76280-91-6, C14H5C16NO3). purity is greater than or equal to 99%.
4.6 Luteumphthalein Standard Stock Solution. Accurately weigh an appropriate amount of Luteumphthalein standard material, and prepare a standard stock solution with a concentration of 1mg/mL with methanol.
Prepare the solution and store it in a refrigerator at -18 ° C.
4.7 Luteumphthalein Standard Intermediate Solution. Accurately absorb an appropriate amount of Luteumphthalein standard stock solution (4.6), prepare a standard intermediate solution with a concentration of 100 μg/mL with methanol, and store in a refrigerator at 0 ° C to 4 ° C.
4.8 Blank sample matrix solution. Select a sample that does not contain the analyte, and follow steps 7.1 and 7.2 to obtain a blank sample matrix solution.
4.9 Luteum phthalate standard matrix solution. As needed, a suitable amount of Luteum phthalate standard intermediate solution (4.7) is pipetted, and a blank sample matrix is used for dissolution.
The solution (4.8) was prepared into a standard matrix solution of appropriate concentration, stored in a refrigerator at 0 ° C to 4 ° C, and prepared before use.
5 instruments and equipment
5.1 Liquid chromatography-tandem mass spectrometer. equipped with an electrospray ion source.
SN/T 1017.6-2019
5.2 Balance. Sensitivity of 0.1mg and 0.01g.
5.3 Oscillator.
5.4 Food grinder.
5.5 Solid-phase extraction column. Sep-PakC18 (60mg, 3mL), or equivalent. Before use, activate with 10mL methanol and 10mL water in sequence.
5.6 Glass suction filter bottle.
5.7 Erlenmeyer flask. 250mL.
6 Sample preparation and storage
6.1 Sample preparation
Take a representative sample of about 500g (not washable with water), chop the edible part, mix thoroughly and put it in a food grinder
Crushed, packed in clean containers, sealed and marked.
6.2 Sample preservation
During sample preparation, sample contamination or changes in residue content should be prevented. Store the samples in the dark below 4 ° C.
7 Measurement steps
7.1 Extraction
Weigh a 10g sample (accurate to 0.01g) into a 500mL conical flask, add 20mL of water, and let stand for 2h. Add 100mL of methanol,
Shocked for 30 minutes. Filter with 1cm diatomaceous earth. Add 50mL and 30mL of methanol to the Erlenmeyer flask respectively.
Filter with 1cm diatomaceous earth on the filter paper, and combine the filtrate in a 250mL Erlenmeyer flask.
7.2 purification
After the above solution was transferred to a purification column (5.5), the first 10 mL of effluent was discarded, and the 5 mL of effluent after collection was collected for liquid chromatography-tandem
Spectrometer determination and confirmation.
7.3 Determination
7.3.1 Liquid chromatography conditions
The liquid chromatography conditions are as follows.
a) Chromatographic column. ElipsePlusC18 column, 50mm × 2.1mm, 1.8μm, or equivalent;
b) Column temperature. 30 ° C;
c) injection volume. 10 μL;
d) flow rate. 0.3mL/min;
See Table 1 for mobile phase and gradient elution conditions.
SN/T 1017.6-2019
Table 1 Mobile phase and gradient elution conditions
time
(Min) Methanol (%)
0.1% formic acid aqueous solution
(%)
0.0 40 60
0.5 40 60
2.5 95 5 5
4.5 95 5 5
4.6 40 60
6.0 40 60
7.3.2 Mass spectrometry reference conditions
The mass spectrometry conditions are as follows.
a) Ionization method. Electrospray ionization (ESI);
b) scanning method. negative ion scanning;
c) Detection method. multiple response monitoring (MRM);
d) Electrospray voltage. 2400V;
e) The sheath gas and auxiliary gas are both high-purity nitrogen, and the collision gas is high-purity argon. The gas flow should be adjusted before use to achieve mass sensitivity
For testing requirements, see Appendix A for reference conditions.
f) Monitoring ion pairs (m/z). 399.9/212.8 (quantitative ions), 399.9/185.9.
7.3.3 Detection and confirmation of liquid chromatography-tandem mass spectrometry
According to the content of the test sample liquid in the sample, select the concentration of the response value of the test object within the linear response range of the instrument for measurement, such as
If it exceeds the linear response range of the instrument, it should be diluted. The reference retention time of cumene in the above chromatographic conditions is about 3.9 min.
See Appendix B for liquid selective ion chromatograms. Determine the sample and standard working solution according to the conditions of liquid chromatography-tandem mass spectrometry.
The deviation between the retention time of the substance and the retention time of the test substance in the standard solution is within ± 2.5%. The standard curve method was used for quantitative determination.
The characterization should be consistent with the relative abundance of a standard working solution of comparable concentration. The allowable deviation of relative abundance does not exceed the range specified in Table 2.
It can be judged that the corresponding test object exists in the sample.
Table 2 Maximum allowable deviation of relative ion abundance during qualitative confirmation
Relative ion abundance > 50 > 20 ~ 50 > 10 ~ 20 ≤10
Allowable relative deviation ± 20 ± 25 ± 30 ± 50
7.4 Blank experiment
Except that the sample is not weighed, the above steps are performed.
8 Calculation and presentation of results
Chromatographic data processing software or formula (1) is used to calculate the cumene residue in the sample. The blank value should be deducted from the calculation result.
SN/T 1017.6-2019
In the formula.
X --- the residual amount of cumene in the sample, the unit is milligram per kilogram (mg/kg);
犮 --- the concentration of cumene solution obtained from the standard curve, in micrograms per milliliter (μg/mL); 犞 --- the volume of the final sample solution, in milliliters (mL);
Note. The blank value is subtracted from the calculation result.
9 Limit of quantitation and recovery
9.1 Limit of quantitation
The limit of quantification of this method is 0.01 mg/kg.
9.2 Determination of concentration range and recovery rate
The experimental data of the concentration and recovery of this method are shown in Table 4.
Table 3 Recovery ranges of different levels of cumene in brown rice
Matrix name addition level recovery range /%
brown rice
0.01 mg/kg 88.3 to 105.1
0.20 mg/kg 89.9 to 107.3
0.40 mg/kg 81.6 to 101.4
wheat
0.01 mg/kg 94.2 to 102.5
0.20 mg/kg 89.1 to 105.1
0.40 mg/kg 92.5 to 104.2
corn
0.01 mg/kg 93.6 to 106.1
0.20 mg/kg 93.6 to 105.3
0.40 mg/kg 89.5 to 103.2
Lentils
0.01 mg/kg 91.6 to 105.6
0.20 mg/kg 84.6 to 100.5
0.40 mg/kg 92.6 to 99.1
Second method gas chromatography
10 Method summary
Xanthophyll in the sample was extracted with acetone. After liquid-liquid partition purification and extraction, the molecule was dehydrated with anhydrous acetic acid and derivatized.
It is imidyl cumene, followed by liquid-liquid partition with sodium chloride aqueous solution and n-hexane, and purification by silica gel column. Gas Chromatograph-Electron Capture Detection
Device, external standard method.
11 Reagents and materials
Unless otherwise specified, the reagents used are of analytical grade, and the water is first-grade water specified in GB/T 6682.
SN/T 1017.6-2019
13 Sample Preparation and Storage
13.1 Sample preparation
The sample is reduced to 1kg by the quarter method, all ground and passed through a 20-mesh sieve, mixed, divided into two parts, and packed into clean containers.
As a sample, seal and mark.
13.2 Sample preservation
Store the sample at -5 ° C or lower in the dark.
Note. During the operation of sampling and sample preparation, prevent the sample from being contaminated or changing the content of residues.
14 Measurement steps
14.1 Extraction
Weigh about 10g of the sample (accurate to 0.01g) into a 250mL conical flask, add 20mL of water, and let it stand for 2h. Add 100mL of acetone,
Swing for 30 min. Filter with 1cm diatomaceous earth. Add 50mL of acetone to the Erlenmeyer flask and apply 1cm of diatomaceous earth with the above.
Filter paper was used for suction filtration, and the filtrates were combined in a 250 mL pear-shaped bottle, and concentrated by rotation at 40 ° C in a water bath to about 20 mL.
The above solution was washed into a 250 mL separatory funnel with 100 mL of a 5% sodium chloride aqueous solution and 50 mL of ethyl acetate, and shaken.
After 5 min, the layers were separated and the ethyl acetate layer was transferred to another 250 mL Erlenmeyer flask. The same operation was performed with 50 mL of ethyl acetate. merge
The filtrate was added with 20 g of anhydrous sodium sulfate and shaken, and then filtered into a 250 mL pear-shaped bottle. Wash the Erlenmeyer flask and filter paper with 20 mL of ethyl acetate
SN/T 1017.6-2019
The remaining residues were combined in a pear-shaped bottle, and concentrated in a 40 ° C water bath to dryness.
The residue was washed into a 100-mL separatory funnel with 30 mL of n-hexane (11.4) and 30 mL of acetonitrile (11.1), shaken for 5 minutes, and left to stand.
The layers were separated and the acetonitrile layer was retained. Add 30 mL of acetonitrile (11.1) to the n-hexane layer, repeat the above operation, and combine the acetonitrile layers to separate at 125 mL
In the funnel. Add 50mL of n-hexane, shake the 5min acetonitrile layer and transfer to a 250mL pear-shaped bottle, and rotate to concentrate in a 40 ℃ water bath
Related standard:   SN/T 1017.1-2019  SN/T 1017.7-2014
   
 
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