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Food safety national standard -- Determination of permethrin residues in food by gas chromatography-mass spectrometry
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GB 23200.31-2016
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Basic data | Standard ID | GB 23200.31-2016 (GB23200.31-2016) | | Description (Translated English) | Food safety national standard -- Determination of permethrin residues in food by gas chromatography-mass spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 11,146 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 1983-2007 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.31-2016: Food safety national standard -- Determination of permethrin residues in food by gas chromatography-mass spectrometry ---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.
Food safety national standard - Determination of permethrin residues in food by gas chromatography - mass spectrometry
National Standards of People's Republic of China
GB
Instead of SN/T 1983-2007
National standards for food safety
Determination of permethrin residues in foodstuffs
Gas chromatography - mass spectrometry
National food safety standards-
Determination of flumioxazins residues in foods
Gas chromatography - mass spectrometry
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 1983-2007 "Method for the determination of benzalkonium bromide residues in food for import and export by gas chromatography-mass spectrometry".
Compared with SN/T 1983-2007, 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 food" to "food";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 1983-2007.
National standards for food safety
Determination of permethrin residues in food by gas chromatography - mass spectrometry
1 Scope
This standard specifies the preparation of the method for the determination of propafenone residues in food and the method of gas chromatography-mass spectrometry.
This standard applies to apples, spinach, ginger, fish, chicken, pork, soybeans, rice, almonds and liver caffeine residues
Of the quantitative determination of 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 samples were extracted with acetonitrile or ethyl acetate and purified by amino solid phase extraction. The eluate was concentrated and concentrated. The gas chromatography-mass spectrometry
Ion monitoring mode for determination, 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 Acetonitrile (CH3CN). Chromatographically pure.
4.1.2 Toluene (C7H8). Chromatographic pure.
4.1.3 Ethyl acetate (C4H8O2). Chromatographic purity.
4.1.4 n-hexane (C6H14). chromatographic purity.
4.1.5 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, stored in a sealed container for use.
4.2 reagent preparation
4.2.1 acetonitrile saturated n-hexane. take a small amount of acetonitrile added to n-hexane, vigorous shaking, and continue to add acetonitrile to appear obvious stratification, static
For use.
4.2.2 acetonitrile - toluene (3 1). take 300 mL of acetonitrile, add 100 mL of toluene, shake back.
4.3 standards
4.3.1 Propoxifenone (Flumioxazin, CH15FN2O4, CAS.No. 103361-09-7) Standard. Purity > 99%.
4.4 standard solution preparation
4.4.1 propafenone standard solution. accurately weighed the appropriate amount of propafenamine standard, with acetonitrile prepared into a concentration of 100 μg/mL
Standard stock solution, this solution is stored in a brown volumetric flask, 0 ℃ ~ 4 ℃ under the conditions of preservation. Dilute the stock solution with acetonitrile as needed,
Prepared into the appropriate concentration of the standard working fluid, 0 ℃ ~ 4 ℃ under the conditions of preservation.
4.4.2 matrix standard working solution. matrix standard working solution is the appropriate amount of propafenone standard use of liquid, with blank matrix extract
Prepare the appropriate concentration of matrix standard working solution. Matrix standard working solution should be used with the current distribution.
4.5 Materials
4.5.1 LC-NH2 Amino solid phase extraction column. 3 mL, 0.5 g or equivalent.
5 instruments and equipment
5.1 Gas Chromatography-Mass Spectrometer. Equipped with an electron impact source (EI).
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 Rotary Evaporator.
5.4 solid phase extraction device.
5.5 blowing nitrogen enrichment instrument.
5.6 vortex mixer.
5.7 Centrifuge.
5.8 high-speed organization of crusher.
5.9 Concentrated bottles. 250 mL.
5.10 Centrifuge tube. 15 mL, 50 mL.
5.11 Microinjector. 10 μL.
6 Preparation and storage of samples
6.1 Soybeans, rice and almonds
500 g of the sample was taken and pulverized and passed through a sample sieve having a pore size of 2.0 mm. Mixed evenly divided into two,
Into a clean container, sealed and marked; stored at -4 ℃ in dark.
6.2 spinach, apples and ginger
Remove the sample by at least 500 g, cut it into small pieces, homogenize the sample with a tissue mill and mix it evenly into two pieces.
Clean sample bag, sealed and marked; stored at -18 ℃ in dark.
6.3 fish, chicken, pork and liver
Substituting the sample at least 500 g, chopping and homogenizing the sample with a tissue masher, evenly divided into two portions, packed in a clean sample
Bag, sealed and identified; in -18 ℃ dark preservation.
During the operation of the sample preparation, it is necessary to prevent the sample from being contaminated or the change in the content of the residue.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
7 Analysis steps
7.1 Extraction
7.1.1 Soybeans, rice and almonds
Weigh 5 g of sample (accurate to 0.0 1 g) in a 50 mL centrifuge tube and extract with 15 mL of acetonitrile for 3 min,
R/min centrifugation 3 min, the extract into another centrifuge tube, respectively, with 15 mL, 10 mL acetonitrile repeat the above operation once, combined to mention
Take the solution into the centrifuge tube, add 5 mL of acetonitrile saturated n-hexane, shake 2 min, centrifuged at 4 000 r/min 3 min, discarded
Alkane layer. The acetonitrile layer was transferred to a 250 mL concentrated flask, concentrated in a 45 OC water bath under reduced pressure to near dryness, and 2 mL of acetonitrile-toluene (3 1)
Dissolve the residue, to be purified.
7.1.2 Spinach, apples and ginger
Weigh 5 g of sample (accurate to 0.0 1 g) in a 50 mL centrifuge tube, add 5 g of anhydrous sodium sulfate, add 15 mL of ethyl acetate
Take 3 min, centrifuge at 5 000 r/min for 3 min, repeat the above operation twice, merge the supernatant to 250 mL concentrated flask
, Concentrated in a 45 ° C water bath under reduced pressure to near dryness, add 2 mL of acetonitrile-toluene (3 1) to dissolve the residue, to be purified.
7.1.3 fish, chicken, pork and liver
Weigh 5 g of sample (exactly 0.0 1 g) in a 50 mL centrifuge tube, add 5 g of anhydrous sodium sulfate, extract with 15 mL of acetonitrile,
Fully shaken for 3 min, centrifuged at 4 000 r/min for 3 min, the extract into another centrifuge tube, respectively, with 15 mL and 10 mL B
Nitrile The above procedure was repeated once, the extracts were combined, 5 mL of acetonitrile saturated n-hexane was added to the centrifuge tube, shaken for 2 min at 4 000 r/min
After centrifugation for 3 min, the n-hexane layer was discarded. The solution was transferred to a 250 mL eggplant flask and the centrifuge tube was washed twice with 5 mL of acetonitrile and washed
The polyester liquid was combined into a concentrated flask and concentrated in a 45 ° C water bath under reduced pressure to near dryness. Add 2 mL of acetonitrile-toluene (3 1) to dissolve the residue.
The
7.2 Purification
The LC-NH2 amino solid phase extraction column was pre-leached with 5 mL of acetonitrile-toluene (3 1). The extract was poured into the extraction column and 12 mL
Acetonitrile-toluene (3 1) was injected into an extraction column and eluted to collect the eluent. The solvent was purged with nitrogen in a water bath at 45 ° C with toluene
Dissolved and fixed to 1.0 mL, gas chromatography - mass spectrometry.
7.3 Determination
7.3.1 Gas Chromatographic Reference Conditions
A) Column. DB-5MS quartz capillary column, 30 m 0.25 mm (id) 0.25 m, or equivalent;
B) Carrier gas. helium, purity greater than or equal to 99.995%; constant current mode, flow rate 1.0 mL/min;
C) Column temperature conditions. 60 ℃ (2 min) 15 ℃/min 300 ℃ (10 min);
D) Inlet temperature. 320 ° C.
E) Injection method. No split injection. After 1 min, open the diverter valve.
F) Injection volume. 2 μL.
7.3.2 Mass spectrometry reference conditions
A) Ion source temperature. 230 ° C
B) Transmission line temperature. 300 ° C
C) ionization mode. EI
D) ionization energy. 70eV
E) Select the monitoring ion (m/z). 259,287,325,354.
7.3.3 Qualitative determination
Under the above chromatographic conditions, the retention time of propafenone was about 19.9 min, and the retention time of the compound peaks in the sample to be tested
The range of variation should be within ± 0.25 min compared to the standard solution.
In the sample mass spectrum after subtracting the background, the relative abundance of the ions in the monitored ions was chosen to be higher than that of the standard samples of propofluorfen
Should be consistent, the similarity within the tolerance, see Table 1. The spectrum of the standard spectrum of propafenone is shown in Figures A.1 and A.2 in Appendix A.
Table 1 Comparison of the relative abundance ratio and maximum allowable deviation of phenanthroline
Compound Qualitative ion (m/z) Relative abundance ratio (%) Allowable relative deviation (%)
354.00 100 /
325.00 10 ± 50
287.00 33 ± 25
259.00 18 ± 30
7.3.4 Quantitative determination
This method uses the external standard method to quantify the quantitative ion m/z354. In order to reduce the effect of matrix on quantification, we need blank sample to prepare
Using the standard working solution of the matrix, according to the sample solution of propafenone out of the peak, select the response value of similar matrix standard working solution
Quantitative, standard working fluid and sample volume of the same method of plug-in measurement, the standard working solution and sample solution of propafenone in the response value should be in the instrument
Detection within the linear range.
7.4 blank experiment
In addition to the sample, according to the above determination steps.
8 results are calculated and expressed
Use the chromatographic workstation or calculate the content of propafenone in the sample by the following formula (1). The calculated result shall be deducted from the blank value.
A c V
X = (1)
AS m
Where.
X - The content of propafenone in milligrams per kilogram (mg/kg);
A - the peak area of propafenone in the sample;
AS-matrix standard solution of propafenone peak area;
C - matrix standard solution concentration in milligrams per liter (mg/L);
V - the final volume of the sample solution, in milliliters (mL);
M - sample sample volume, unit g (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 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 quantification limit of this method is. 0.01 mg/kg.
10.2 Recovery rate
The experimental data on the concentration and recovery of propafenone are shown in Appendix B.
Appendix A
(Informative)
Standard ion chromatogram
Figure A.1 Acetylfluorfenamine standard ion chromatogram
Figure A.2 Propofluorfenamine Standard EI Full Scanning Mass Spectrometry
50 100 150.200 250 300 350 400 450 500 550
M/z - >
Abundance
176 52 406 152 129 232 382 578 430 515 470 551 492
Appendix B
(Informative)
Sample concentration and recovery of the experimental data
Table B.1 Experimental data on the concentration and recovery of the sample
Sample name Add concentration, μg/kg Recovery (%)
Rice
10 84.5 98.6
20 91.0102.0
200 95.0 102.5
Soybeans
10 80.3 88.6
20 83.5 95.5
200 88.094.5
spinach
10 73.4 89.6
20 94.0 100.5
200 88.0 100.5
apple
10 88.1 99.6
20 91.597.0
200 90.5 99.5
almond
10 78.5 92.2
20 87.5 95.0
200 86.092.0
pork
10 87.8 94.3
20 92.5 105.0
200 86.0 93.5
chicken
10 85.6 94.1
20 90.5 107.0
200 88.5 94.0
10 75.8 92.8
20 96.5 105.5
200 94.5 100.0
Liver
10 74.1 82.1
20 82.5 91.5
200 87.095.0
10 73.482.3
20 82.5 90.5
200 78.5 87.5
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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