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GB 23200.72-2016: Food safety national standard -- Determination of benzamide residues in foodstuffs by gas chromatography-mass spectrometry
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Food safety national standard -- Determination of benzamide residues in foodstuffs by gas chromatography-mass spectrometry
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GB 23200.72-2016
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Basic data | Standard ID | GB 23200.72-2016 (GB23200.72-2016) | | Description (Translated English) | Food safety national standard -- Determination of benzamide residues in foodstuffs by gas chromatography-mass spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 16,138 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 3143-2012 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.72-2016: Food safety national standard -- Determination of benzamide residues in foodstuffs by gas chromatography-mass spectrometry
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Food safety national standard - Determination of benzamide residues in foodstuffs by gas chromatography - mass spectrometry
National Standards of People's Republic of China
GB
Replace SN/T 3143-2012
National standards for food safety
Determination of Benzamide Pesticide Residues in Food
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 Food and Drug Administration
Foreword
This standard replaces SN/T 3143-2012 "Determination of benzamide pesticide residues in export food by gas chromatography-mass spectrometry".
Compared with SN/T 3143-2012, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- the name and scope of the "export food" to "food";
- Add "other food can refer to execution" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 3143-2012
National standards for food safety
Determination of benzamide residues in foodstuffs by gas chromatography - mass spectrometry
1 Scope
This standard specifies the method of gas chromatography-mass spectrometry for the determination of 25 benzamide pesticide residues in foodstuffs (see Appendix A).
This standard applies to corn, spinach, mushrooms, apples, soybeans, chestnuts, tea, beef, beef liver, chicken, fish, milk
25 kinds of benzamide pesticide residues in the determination and confirmation, 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 date of the date applies to this
file. For undated references, the latest edition (including all modifications) applies to this document.
GB 2763 National Standard for Food Safety - Maximum Residue Limits for Pesticides in Foodstuffs
GB/T 6682 Analytical laboratory water specifications and test methods
3 principle
The samples were extracted with acetone-n-hexane, extracted with graphitized carbon black solid phase extraction column or neutral alumina solid phase extraction column. Gas chromatography-
Mass spectrometer determination and confirmation, external standard method quantitative.
4 reagents and materials
Unless otherwise specified, all reagents are of analytical grade and the water is in accordance with the primary water specified in GB/T 6682.
4.1 Reagents
4.1.1 n-hexane (C6H14). pure chromatography.
4.1.2 Acetone (CH3COCH3). Chromatographic pure.
4.1.3 Sodium chloride (NaCl).
4.1.4 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, set the dryer in the spare.
4.2 solution preparation
4.2.1 Acetone-n-hexane solution (1 2, V/V). Take 100 mL of acetone, add.200 mL of n-hexane and shake well.
4.2.2 acetone - n-hexane solution (1 1, V/V). take.200 mL of acetone, add.200 mL of n-hexane, shake back.
4.3 standards
4.3.1 Benzamide Pesticide Reference Material. See Appendix A.
4.4 standard solution preparation
4.4.1 benzamide pesticide standard stock solution. were accurately weighed appropriate amount of benzamide pesticide standard substances, with acetone prepared into 1 000
μg/mL standard stock solution, the standard solution away from 0 ℃ ~ 4 ℃ preservation, shelf life of 6 months.
4.4.2 benzamide pesticide standard working solution. According to the testing requirements, respectively, the amount of the standard stock solution in the same capacity bottle, with
N-hexane diluted to the standard preparation of the appropriate concentration of the standard working solution, the standard solution away from 0 ℃ ~ 4 ℃ preservation, shelf life of one month.
4.5 Materials
4.5.1 Graphitized Carbon Black Solid Phase Extraction Column. 6 mL 500 mg, or equivalent.
4.5.2 Neutral Alumina Solid Phase Extraction Column. 6 mL 500 mg, or equivalent.
5 instruments and equipment
5.1 Gas Chromatography-Mass Spectrometer, with electron bombardment ion source (EI source).
5.2 Tissue crusher.
5.3 Crusher.
5.4 Analytical balance. 0.01 g and 0.0001 g.
5.5 Scroll Mixer.
5.6 solid phase extraction device with vacuum pump.
5.7 Centrifuge. 6 000 r/min.
5.8 Centrifuge tube. 50 mL.
5.9 scale tube. 15 mL.
5.10 Microiner. 10 μL.
6 Preparation and storage of samples
6.1 Sample preparation
6.1.1 Fruits, mushrooms or vegetables
Take a representative sample of 500 g, after shredding (not available in water), and the sample is processed into a slurry using a crusher. Mix well and put it clean
Within the sample container, seal and mark the mark.
6.1.2 tea, soybeans, chestnut, corn
Take a representative sample 500 g, crushed with a pulverizer. Mix, fit into a clean container, sealed and marked.
6.1.3 Milk
Mix the sample evenly and separate 500 g as a sample. The prepared samples were divided into two separate sections, which were sealed in a vial and sealed
Mark the mark.
6.1.4 beef, beef liver, fish, chicken
Take a representative sample 500 g, fully mashed by the crusher, into a clean sample container, sealed and marked.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
6.2 Sample storage
Tea, soybeans, chestnuts, cereals and other samples at 0 ℃ 4 ℃ preservation; milk, mushrooms, fruits and vegetables and meat and meat products
And other samples in -18 ℃ below frozen storage.
During sample preparation, the sample should be protected from contamination or changes in residue content.
7 Analysis steps
7.1 Extraction
For tea, soy, chestnut, corn samples, weigh 2.5 g sample (accurate to 0.01 g). For spinach, mushrooms, apples,
Beef, beef, chicken, fish, milk samples, weighed 5 g sample (accurate to 0.01 g). Place the weighed sample in a 50 mL centrifuge tube
, Add 6 mL of saturated aqueous sodium chloride solution, mix on a vortex mixer for 30 s for 15 min. Add 6 mL of acetone-n-hexane solution,
Mix on a mixer for 2 min. 5 000 r/min centrifugation 1 min, absorb the upper extract in another tube. And then add 4 mL of acetone -
The n-hexane solution was repeatedly extracted twice and the extracts were combined and the nitrogen stream was blown to about 1 mL at 45 ° C to be purified.
7.2 Purification
7.2.1 Tea, spinach, mushrooms, apples
A graphitized carbon black solid phase extraction column (1 cm high anhydrous sodium sulfate layer in the column) was mounted on a solid phase extraction vacuum suction apparatus,
The extraction column was pre-eluted with 6 mL of acetone-n-hexane (4.2.2) and the whole pre-eluent was discarded. The extract was added to the graphitized carbon black solid phase
In the extraction column, the extract was completely eluted and the extract was eluted with 8 mL of acetone-n-hexane mixture to maintain a flow rate of 1.5 mL/min.
The whole effluent was collected and the nitrogen stream was blown to near dry at 45 ° C. With constant volume of n-hexane to 0.5 mL for GC-MS determination.
7.2.2 corn, soybeans, chestnut, beef, beef liver, chicken, fish, milk
A neutral alumina solid phase extraction column (1 cm high anhydrous sodium sulfate layer in the column) was mounted on a solid phase extraction vacuum suction apparatus,
First with 6 mL of acetone - n-hexane mixture pre-elution extraction column, discard all pre-eluent. The extract was added to neutral alumina for solid phase extraction
In the column, the extract was completely eluted and the extract was eluted with 5 mL of acetone-n-hexane mixture to maintain a flow rate of 1.5 mL/min.
The whole effluent was blown to near dry at 45 ° C. With constant volume of n-hexane to 0.5 mL for GC-MS determination.
7.3 Determination
7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions
a) Column. HP-1701MS quartz capillary column, 30 m 0.25 mm (id), film thickness 0.25 m, or equivalent.
b) Column temperature. 100 ° C (for 1 min) 10 ° C/min 280 ° C (for 11 min).
c) Inlet temperature. 250 ° C.
d) chromatographic - mass spectrometer interface temperature. 280 ° C.
e) Carrier gas. helium, purity greater than or equal to 99.995%, 1.0 mL/min.
f) Injection volume. 1 μL.
g) Injection method. no split injection, 1 min after the valve.
h) ionization mode. EI.
i) Ionization energy. 70 eV.
j) Detection method. Select the ion monitoring mode (SIM).
k) Monitoring ions (m/z). See Appendix A.
l) solvent delay. 8 min.
7.3.2 Determination and confirmation of chromatography
According to the content of benzamide pesticide in the sample solution, the standard working solution with similar peak area is selected, and the standard working solution and sample solution
Volume of the plug-in sample, the standard working solution and sample solution of benzamide pesticide response value should be in the instrument within the linear range.
Under the same experimental conditions, the mass retention time of the substance to be tested in the sample was the same as that of the standard working solution and the sample was subtracted from the background
The mass of the selected ions in the mass chromatogram is compared with the abundance of the selected ions compared to the abundance of the corresponding ions of the standard.
(The allowable range in Table 1) can determine the existence of the corresponding sample in the sample. Under the above chromatographic conditions, the retention of benzamide pesticides
Time and its monitoring of the ion (m/z) abundance ratio see Appendix A. The total ion chromatogram and mass spectrum of the standard are shown in Appendix B, Figure B.1 and attached
Record C in Figure C.1
Table 1 Maximum allowable error for relative ion abundance using gas chromatography-mass spectrometry
7.4 blank experiment
In addition to the sample, according to the above determination steps.
8 results are calculated and expressed
Use the chromatographic data processor or calculate the content of each benzamide pesticide in the sample according to the following formula (1).
Where.
X - Residual content of benzamide pesticide in the sample in milligrams per kilogram, mg/kg;
The peak area of benzamide pesticides in sample solution;
V - the final volume of the sample solution, in milliliters, mL;
Asi - the peak area of benzamide pesticides in standard working fluids;
Csi - the concentration of benzamide pesticides in standard working fluids in micrograms per milliliter, g/mL;
m - the amount of sample represented by the final sample, 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 reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix E requirements.
9.2 The ratio of the absolute difference between the two independent measurements obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix F requirements.
10% limit and recovery rate
10.1 Limit of limits
The limit of quantification of the benzamide pesticide is 0.01 mg/kg.
10.2 Recovery rate
The addition rates of 25 benzamide pesticides are shown in Appendix D when the levels are 0.01 mg/kg, 0.05 mg/kg, 0.2 mg/kg.
Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10%
Allowable relative deviation ± 20% ± 25% ± 30% ± 50%
Appendix A
(Informative)
The CAS number, retention time and monitoring ion abundance ratio of 25 benzamide pesticides
Table A.1 CAS number, retention time and monitoring ion abundance ratio of 25 benzamide pesticides
Appendix B
(Informative)
A total of total amino acid chromatograms of standard compounds for benzamide
Figure B.1 Total ion chromatogram of 25 benzamide pesticide reference materials
Appendix C.
(Informative)
25 standard spectrum of benzamide pesticide standard
Figure C.1 Standard spectrum of 25 benzamide pesticides
Appendix D
(Informative)
Addition recovery of 25 benzamide pesticides in different matrices
Table D.1 Recovery rates of 25 benzamide pesticides in different matrices
Appendix F
(Normative appendix)
Inter-laboratory reproducibility requirements
Table F.1 Inter-laboratory reproducibility requirements
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