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GB 23200.36-2016: Food safety national standard -- Determination of chloroplopidic acid, fenpropathrin, furazolidone and thiazole niacin herbicide residues in plant-derived foods by liquid chromatography-mass spectrometry / mass spectrometry
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Food safety national standard -- Determination of chloroplopidic acid, fenpropathrin, furazolidone and thiazole niacin herbicide residues in plant-derived foods by liquid chromatography-mass spectrometry / mass spectrometry
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GB 23200.36-2016
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Basic data | Standard ID | GB 23200.36-2016 (GB23200.36-2016) | | Description (Translated English) | Food safety national standard -- Determination of chloroplopidic acid, fenpropathrin, furazolidone and thiazole niacin herbicide residues in plant-derived foods by liquid chromatography-mass spectrometry / mass spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 11,181 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 2214-2008 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.36-2016: Food safety national standard -- Determination of chloroplopidic acid, fenpropathrin, furazolidone and thiazole niacin herbicide residues in plant-derived foods by liquid chromatography-mass spectrometry / mass spectrometry
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Food safety national standard - Determination of chloroplopidic acid, fenpropathrin, furazolidone and thiazole niacin herbicide residues in plant-derived foods by liquid chromatography-mass spectrometry/mass spectrometry
National Standards of People's Republic of China
GB
Instead of SN/T 2214-2008
National standards for food safety
Plant-derived food chlorofluoropyoxyacetic acid, fenpropathrin,
Determination of vanillin hydrazone and thiazole niacin herbicide residues
Liquid chromatography - mass spectrometry/mass spectrometry
National food safety standards-
Determination of fluroxypyr, dithiopyr, diflufenzopyr and thiazopyr
Residues in plant-derived foods
Liquid 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 2214-2008 "Flavonoids, Fluorothiocuronide, Fipronil and Hydrazone Herbicides in Import and Export Plant Foods
Determination of Residue by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry ".
Compared with SN/T 2214-2008, 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 of plant-derived food" to "plant-derived food";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 2214-2008.
National standards for food safety
Flavulanic acid, fenpropathrin, furazolidone and thiazole niacin in plant-derived food
Determination of residual residue by liquid chromatography - mass spectrometry/mass spectrometry
1 Scope
This standard specifies the chlorpyrifluoroacetic acid, fenpropathrin, fluphenhydrazone and thiazole nicotinic acid in the plant source food.
Determination of Chromatography - Mass Spectrometry/Mass Spectrometry.
This standard applies to cabbage, corn and oranges in the chlorofluoropyoxyacetic acid, fenpropathrin, fenugreeosone and thiazole nicotinic acid four kinds of pyridine
Determination and determination of herbicide residues, 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 residual chlorofluoropyoxyacetic acid in the sample, fenpropathrin, furazolidone and thiazole niacin were extracted with acetonitrile and purified by Supelclean C18 solid
Phase extraction column, with liquid chromatography - mass spectrometry/mass spectrometry detection and confirmation, 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 Methanol (CH3OH). Chromatographic Purification.
4.1.3 Formic acid (HCOOH). Chromatographic pure.
4.1.4 Sodium chloride (NaCl).
4.2 solution preparation
4.2.1 0.1% formic acid in water solution. Accurately absorb 1 mL of formic acid, transfer into a 1 000 mL volumetric flask, set the volume to the mark with water, mix
Evenly.
4.2.2 0.1% formic acid - methanol (50 50, V/V). Take 0.1% formic acid as an aqueous solution 500 mL to 1 000 mL volumetric flask.
Methanol constant volume to the scale, mixed evenly.
4.3 standards
4.3.1 Pyridine Herbicides Standard. See Appendix A.
4.4 standard solution preparation
4.4.1 standard reserve solution. accurately weighed the appropriate amount of chlorofluorophenoxy acetic acid, fenpropathrin, thiazole nicotinic acid were dissolved with methanol and volume to
Brown volumetric flask, the concentration is equivalent to 500 mg/L, the stock solution can be stored at 0 ℃ ~ 4 ℃ dark for 6 months.
4.4.2 mixed standard intermediate solution. accurate absorption of the appropriate amount of chlorofluoropyoxy acetic acid, fenpropathrin, thiazole niacin standard reserve solution in brown capacity
And the addition of other pyridine herbicides and other concentrations of picarbazone hydrazone, with a fixed volume of methanol to the scale, a variety of pyridine herbicides
Concentration of 1 mg/L, the intermediate solution can be stored at 0 ℃ ~ 4 ℃ dark for 1 month.
4.4.3 mixed standard working solution. according to need, before use to absorb a certain amount of mixed standard intermediate solution, with a blank sample matrix solution
Preparation.
4.5 Materials
4.5.1 Solid phase extraction column. Supelclean C18,500 mg/3 mL, or equivalent. Before use with 5 mL acetonitrile treatment, keep the column wet
Run.
4.5.2 Microporous membrane. 0.22 μm, organic phase type.
5 instruments and equipment
5.1 Liquid Chromatography - Mass Spectrometry/Mass Spectrometer with ESI Ion Source.
5.2 Balance. 0.0001 g and 0.01 g.
5.3 Crusher.
5.4 Polypropylene centrifuge tube. 15 mL and 50 mL, with plug.
5.5 Centrifuge. 5 000 r/min.
5.6 Scroll Mixer.
5.7 blowing nitrogen enrichment instrument.
5.8 solid phase extraction device.
6 Preparation and storage of samples
6.1 Preparation of the sample
6.1.1 Chinese cabbage and oranges
Take about 500 g of the sample, (not water wash). After shredding, the sample is processed into a slurry, mixed,
Sealed, marked and marked.
6.1.2 Corn
Replace the sample about 500 g, fully crushed, mix, into a clean container, sealed and marked.
6.2 Sample storage
Samples were stored at 0 ° C and 4 ° C. During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
7. Determination steps
7.1 Extraction
Weigh 5 g (accurate to 0.01 g) sample in a 50 mL centrifuge tube and add proper amount of deionized water for a while. 10 mL of acetonitrile was added,
Mix on a vortex mixer for 3 min, centrifuge at 5000 r/min for 5 min, transfer the supernatant to another centrifuge tube. Respectively, with 10 mL,
5 mL of acetonitrile Repeat the above extraction process and combine the extracts. Add appropriate amount of sodium chloride, full oscillation, centrifugation in 5000 for 3 min. Take 5 mL of the upper layer
Acetonitrile extract to 15 mL centrifuge tube, at 40 ℃ blowing nitrogen concentrated to about 2 mL, fully mixed.
7.2 Purification
The sample extract was transferred to a C18 solid phase extraction column. Eluting with 4 mL of acetonitrile and collecting the entire effluent (approximately 6 mL) from the sample
The solid phase extraction purification process controls the flow rate to no more than 1 d/s. The effluent was blown to near dryness at 40 ° C with 0.1% formic acid-methanol (50 50,
V/V) to 1.0 mL, and the mixture was vortexed and passed through a 0.22 μm microporous membrane for liquid chromatography-mass spectrometry/mass spectrometry.
7.3 Determination
7.3.1 Liquid Chromatography Chromatographic Reference Conditions
A) Column. ACQUITY BEH C18 column, 50 x 2.1 mm (inner diameter), 1.7 μm, or equivalent.
B) Column temperature. 40 ° C.
C) Flow rate. 0.3 mL/min.
D) Injection volume. 20 μL.
E) Flow phase and gradient elution conditions are shown in Table 1.
Table 1 Mobile phase and gradient elution conditions
time
Min
Flow rate
ML/min
0.1% formic acid in water
Methanol
0 0.3 80 20
6 0.3 0 100
7.5 0.3 80 20
7.3.2 Mass spectrometry reference conditions
A) Ionization mode. electrospray ionization positive ion mode (ESI).
B) Resolution. Unit mass resolution.
C) Capillary voltage (kv). 3.00.
D) Source temperature (° C). 105.
E) Desolvation gas temperature (° C). 350 ° C.
F) Desolvent gas flow rate (L/hr). 750.
G) Monitoring mode. Multiple reaction monitoring (MRM), see Appendix A Table A.1 for setting conditions.
7.3.3 Determination and confirmation of chromatography
According to the above conditions to determine the sample and mixed matrix standard solution, the sample retention time of the material to be tested and the substrate standard solution retention
And the relative abundance of the qualitative ion pair is consistent with the relative abundance of the standard solution of the mixed matrix equivalent to the concentration.
Degree deviation does not exceed the provisions of Table 2, you can determine the existence of the corresponding sample in the sample.
In the best working conditions of the instrument, the standard solution of the mixed working solution of the matrix, with the peak area as the ordinate, the matrix mixed working solution concentration
The standard working curve is drawn for the abscissa, and the sample is quantified by the standard working curve. The response value of the sample to be measured in the sample solution should be
Determination of the linear range. Under the above liquid chromatography-mass/mass spectrometry conditions, chlorofluorophenoxyacetic acid, fluphenhydrazone, fenpropathrin and thiazole
The retention time of nicotinic acid is given in Appendix A, Table A.1. Total Ion Flow Chromatography and Multiple Reaction Monitoring (MRM) of Four Pyridine Herbicides Reference Materials
See Appendix B, Figure B.1 and Figure B.2 for chromatograms.
Table 2 The maximum allowable deviation of relative ion abundance when qualitative confirmation
Relative ion abundance > 50% > 20% to 50% > 10% to 20% ≦ 10%
Maximum permissible deviation ± 20% ± 25% ± 30% ± 50%
7.4 blank experiment
In addition to the sample, according to the above determination steps.
8 results are calculated and expressed
The contents of the four pyridine herbicides in the sample were calculated according to the following formula (1).
MΑs
VCsA
(1)
Where.
The content of four pyridine herbicides in the X - sample, in micrograms per kilogram, μg/kg;
The peak area of pyridine herbicide in A - sample solution;
As - standard working solution of pyridine herbicides peak area;
Cs - four pyridine herbicides from standard working curves in micrograms per liter, μg/L;
V - the final volume of the sample solution, in milliliters, mL;
M - the final sample quality of the 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 D 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 E requirements.
10% limit and recovery rate
10.1 Quantitation limits
The limits of quantification of Chinese cabbage and orange substrate. chlorofluoropyoxyacetic acid, fenpropathrin, fluphenazine and thiazole nicotinic acid were 5 μg/kg;
The limit of quantification of corn matrix. chlorofluoropyoxyacetic acid and fluphenhydrazone is 10 μg/kg, and the limit of quantification of fenpropathrin and thiazole nicotinate is 5
Μg/kg.
10.2 Recovery rate
In the range of 0.005 mg/kg to 0.04 mg/kg, the recovery rates of the four pyridine herbicides are given in Appendix C.
Appendix A
(Informative)
Basic information, retention time and mass spectrometry parameters of four pyridine herbicides
Table A.1 Basic information, retention time and mass spectral parameters of four pyridine herbicides
Pesticide Chinese
name
Pesticide English name
CAS number Molecular formula Molecular weight
Reserved
time
Min
Mother ion
M/z
Ion
M/z
Retention time
Cone hole voltage
Collision energy
EV
Chlorofluorophenoxy
Acetic acid
Fluroxypyr C7H5Cl2FN2O3 69377-81-7 255.03 2.85 255
209 * 0.2 30 15
181 0.2 30 20
2 Fluoropyrazone diflufenzopyr C15H12F2N4O3 109293-97-2 334.28 3.50 335
206 * 0.2 30 15
162 0.2 30 15
3 Fisulfuride dithiopyr C15H16F5NO2S2 97886-45-8 401.41 5.25 402
354 * 0.05 30 18
272 0.05 30 30
4 thiazole niacin thiazopyr C16H17F5N2O2S 117718-60-2 396.37 4.81 397
377 * 0.2 30 21
335 0.2 30 29
Note. * Quantitative detection of ions. For different mass spectrometry instruments, there may be differences in instrument parameters, and the mass spectrometry parameters should be optimized to the best.
Appendix B
(Informative)
The total ion chromatogram of the standard and the multi - reaction monitoring (MRM) chromatogram
Figure B.2 5 μg/L pyridine herbicide standard multi-reaction monitoring (MRM) chromatogram
Figure B.1 5 μg/L pyridine herbicide standard total ion chromatogram
1. chlorofluoropyoxyacetic acid; 2. fluphenhydrazone; 3. thiazole niacin; 4. fenpropathrin.
Chlorofluorophenoxyacetate
Thiazole nicotinic acid thiazole niacin
Fluoride Sulfonated Fenpropathrin
Appendix C
(Informative)
Addition Recovery of Four Pyridine Herbicides in Different Substrates
Table C.1 Recovery rates of four pyridine herbicides in different matrices
No. pesticide name
Sample matrix
Cabbage oranges
Chlorofluorophenoxy
Acetic acid
89.4% ~ 117.8% 86.4% ~ 119.4% 63.5% ~ 117.5%
2 Fluoropyrazine 79.8% ~ 120.0% 71.4% ~ 112.2% 65.7% ~ 122.3%
3 Fisulfurism 60.5% ~ 94.0% 78.4% ~ 115.7% 76.7% ~ 118.0%
4 thiazole niacin 98.0% ~ 112.0% 80.4% ~ 103.0% 84.6% ~ 111.0%
Appendix D
(Normative appendix)
Laboratory repeatability requirements
Table D.1 Laboratory repeatability requirements
Measured component content
Mg/kg
Precision
0.001 36
> 0.01
> 1 14
Appendix E
(Normative appendix)
Inter-laboratory reproducibility requirements
Table E.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
Precision
0.001 54
> 0.01
> 1 19
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