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GB 23200.3-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 3: Determination of cyclohexanone herbicides in food by liquid chromatography-mass spectrometry / mass spectrometry
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Food safety national standard -- Methods for the determination of herbicide residues -- Part 3: Determination of cyclohexanone herbicides in food by liquid chromatography-mass spectrometry / mass spectrometry
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GB 23200.3-2016
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Basic data | Standard ID | GB 23200.3-2016 (GB23200.3-2016) | | Description (Translated English) | Food safety national standard -- Methods for the determination of herbicide residues -- Part 3: Determination of cyclohexanone herbicides in food by liquid chromatography-mass spectrometry / mass spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 20,224 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 1737.3-2010 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No.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 23200.3-2016: Food safety national standard -- Methods for the determination of herbicide residues -- Part 3: Determination of cyclohexanone herbicides in food by liquid chromatography-mass spectrometry / mass spectrometry
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Food safety national standard - Methods for the determination of herbicide residues - Part 3. Determination of cyclohexanone herbicides in food by liquid chromatography - mass spectrometry/mass spectrometry
National Standards of People's Republic of China
GB
Instead of SN/T 1737.3-2010
National standards for food safety
Method for determination of herbicide residue
Part 3. Determination by liquid chromatography - mass spectrometry/mass spectrometry
Residues of Cyclohexenone Herbicides in Food
National food safety standards-
Determination of cyclohexanediones herbicide residues in 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 1737.3-2010 "Methods for the determination of herbicide residues Part 3. Determination by liquid chromatography-mass spectrometry
Export of cyclohexene ketone herbicide residues ".
Compared with SN/T 1737.3-2010, 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 1737.3-2010.
National standards for food safety
Method for determination of herbicide residue
Part 3. Determination of Cyclohexanone in Food by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry
Herbs Residue
1 Scope
This standard specifies the food in the pyranosone, grass grass, thiadenone, oxadiazone, alkenopyridine, butanone, trimethoprostenone, cyclophen
Determination of Ketone Residue by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry.
This standard applies to rice, soybeans, pork, beef liver, chicken liver, milk, oranges, blueberries, spinach, onions, walnuts, tea
Determination of the Residual Amount of Pyrrithione, Herbicide, Thiomethoxone, Cenotrocerone, Energeno,
And confirmed that 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 cyclohexenone herbicides in the sample were extracted with acidic acetonitrile or acetonitrile, and the extract was treated with N-propyl ethylenediamine (PSA), octadecane
(ODS) and graphitized carbon black were purified by liquid chromatography-mass spectrometry/mass spectrometry and quantified by external standard method.
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 Acetic acid (CH3COOH) (99.5%).
4.1.3 Formic acid (HCOOH) (88.0%).
4.1.4 Sodium acetate (CH3COONa).
4.1.5 Sodium chloride (NaCl).
4.1.6 anhydrous magnesium sulfate (MgSO4). 650 ℃ burning 4 h, placed in the dryer to spare.
4.2 solution preparation
4.2.1 1% acetic acid acetonitrile solution. take 10 mL of acetic acid, add 990 mL of acetonitrile, mix.
4.2.2 60% acetonitrile aqueous solution. take 60 mL of acetonitrile, add 40 mL of water, mix.
4.2.3 Formic acid - Aqueous solution (0.2 999.8, V/V). Take 0.2 mL of formic acid, dissolve with water and dilute to 1000 mL.
4.3 standards
4.3.1 Cyclohexenone standards. Clethodim, CAS. 99129-21-2, purity ≥99%; pyranone
(Tepraloxydim) CAS. 149979-41-9, purity ≥99%; thiadenone (Cycloxydim), CAS. 101205-02-1, purity
≥93.5%; Tralkoxydim, CAS. 87820-88-0, purity ≥93.5%; Alloxydim, CAS.
55634-91-8, purity ≥98%; Profoxydim, CAS. 139001-49-3, purity ≥98.5%; butanone
(Butroxydim), CAS. 138164-12-2; Purity ≥99%; Sethoxydim CAS. 74051-80-2; Purity ≥99%.
4.4 standard solution preparation
4.4.1 Cyclohexenone Standard Reserve Solution. Accurately weigh the standard amount of cyclohexenone, dissolve with acetonitrile and set to 100 mL of brown
Color container, the concentration of 100 μg/mL standard stock solution, the solution stored in dark.
4.4.2 mixed standard intermediate solution. accurate extraction of cyclohexene ketone standard stock solution of 2.5mL in 50mL brown volumetric flask, with acetonitrile
Diluted to a concentration of 5.0 μg/mL mixed standard intermediate solution, the solution stored in dark.
4.4.3 Mixing standard working solution. Prepare the appropriate standard working solution with a blank sample matrix prior to use.
4.5 Materials
4.5.1 Graphitized Carbon Black Adsorbent. 120 μm to 400 μm.
4.5.2 N-propyl ethylenediamine (PSA) adsorbent. 40 μm to 100 μm.
4.5.3 Octadecylsilane (ODS) Bonded phase. 40 μm to 100 μm.
4.5.4 Water phase filter. 0.22 μm.
5 instruments and equipment
5.1 LC-MS/MS. ESI ionization source.
5.2 Electronic balance. 0.01 g and 0.0001 g.
5.3 Crusher.
5.4 Tissue crusher.
5.5 Centrifuge. 4 000 r/min.
5.6 vortex mixer.
5.7 nitrogen blowing instrument.
5.8 Homogenizer. 10 000 r/min.
5.9 screw cap polypropylene centrifuge tube. 50 mL, 15 mL.
5.10 glass with a plug centrifuge tube. 15 mL.
6 Preparation and storage of samples
6.1 Preparation of the sample
6.1.1 Oranges, blueberries, spinach, onions
Take a representative sample of about 500 g (can not be washed with water), cut it, and then use the tissue crusher to process the sample into a slurry,
The net container is sealed as a sample, marked and marked.
6.1.2 Soybean, rice, tea, walnut
Approximately 500 g of representative sample, crushed and mixed with a pulverizer, packed in a clean container as a sample, sealed and marked.
6.1.3 pork, bovine liver, chicken liver
Take a representative sample of about 500 g, chopped, with the tissue crusher will be fully mashed evenly, into the clean container as a sample, sealed
And mark the mark.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
6.2 Sample storage
Soybeans, rice, tea, walnut and milk and other samples at 0 ℃ ~ 4 ℃ preservation; oranges, blueberries, spinach, onions, pork,
Chicken liver and other samples stored at -18 ℃ below.
During the operation of the sample preparation, the contamination of the sample or the change in the content of the residue should be prevented.
7 Analysis steps
7.1 Extraction
7.1.1 Soybean, rice, tea and walnut
Weigh the sample 5 g (tea sample 2 g, accurate to 0.01 g) in 50 mL screw cap polypropylene centrifuge tube, add 10 mL of water,
Vortex mixer for 30 min, placed 15 min. Add 3 g of anhydrous magnesium sulfate, 1 g of sodium chloride, 1 g of sodium acetate and 15 mL of 1% acetonitrile solution,
The homogenizer was centrifuged at 10 000 r/min for 2 min and 4 000 r/min for 5 min. The supernatant was transferred to a 25 mL volumetric flask. Reuse
10 mL 1% acetic acid acetonitrile solution to extract once again, the combined extract in the same 25 mL volumetric flask, and acetonitrile volume to the scale, to be purified.
7.1.2 Pork, Bovine Liver, Chicken Liver, Milk, Oranges, Spinach and Onion
Weigh the sample about 5 g (accurate to 0.01 g) in a 50 mL screw cap polypropylene centrifuge tube, add 5 mL of water, 3 g of anhydrous magnesium sulfate, 1 g
Sodium chloride, 1 g of sodium acetate and 15 mL of 1% acetic acid in acetonitrile, homogenized at 10 000 r/min homogenized for 2 min, 4 000 r/min centrifuged 5
Min. The supernatant was transferred to a 25 mL volumetric flask. And then 10 mL 1% acetic acid acetonitrile solution repeated extraction time, combined extract in the same 25 mL
Volumetric flask, and fixed to the scale with acetonitrile, to be purified.
7.1.3 Blueberry
Weigh the sample about 5 g (accurate to 0.01 g) in a 50 mL screw cap polypropylene centrifuge tube, add 5 mL of water, 3 g of anhydrous magnesium sulfate, 1 g
Sodium chloride, 1 g sodium acetate and 15 mL acetonitrile, homogenized at 10 000 r/min homogenization for 2 min and 4 000 r/min for 5 min. Will be on
The supernatant was transferred to a 25 mL volumetric flask. And then 10 mL of acetonitrile repeated extraction time, combined extract in the same 25 mL volumetric flask, and acetonitrile
Constant volume to scale, to be purified.
7.2 Purification
7.2.1 Soybeans, rice, walnuts, pork, beef liver, milk, onions
Remove 8 mL of the above extract in a 15 mL screw cap polypropylene centrifuge tube, add 300 mg of anhydrous magnesium sulfate, 250 mg of PSA and 500 mg
ODS, mixed on a vortex mixer for 2 min, and centrifuged at 4 000 r/min for 5 min. Accurately remove 5 mL of the wash solution in 15 mL glass
Tube, by 60 ℃ nitrogen blowing machine after drying, with 60% acetonitrile aqueous solution and set the volume of 1.0 mL, 0.22 μm filter for liquid chromatography-mass spectrometry
/ Mass spectrometer.
7.2.2 Chicken liver, orange, spinach, blueberry, tea
Remove 8 mL of the above extract in a 15 mL screw cap polypropylene centrifuge tube, add 300 mg of anhydrous magnesium sulfate, 250 mg PSA, 500 mg ODS
And 10 mg of graphitized carbon black were mixed on a vortex mixer for 2 min and centrifuged at 4 000 r/min for 5 min. Accurately remove 5 mL of the purified solution at 15 mL
Glass with a plug centrifuge tube, by 60 ℃ nitrogen blowing machine after drying, with 60% acetonitrile aqueous solution and volume 1.0 mL, 0.22 μm filter for liquid
Determination by mass spectrometry/mass spectrometry/mass spectrometry.
7.3 Determination
7.3.1 Liquid Chromatographic Reference Conditions
7.3.1.1 Column. C18, 50 mm × 2.1 mm (id), particle size 1.7 μm, or equivalent;
7.3.1.2 Mobile phase. see gradient elution program Table 1;
Table 1 gradient elution program table
7.3.1.3 Flow rate. 0.25 mL/min;
7.3.1.4 Column temperature. 30 ° C;
7.3.1.5 Injection volume. 5 μL;
7.3.2 Mass spectrometry reference conditions
See Appendix A.
7.3.3 Liquid Chromatography - Mass Spectrometry/Mass Spectrometry Detection and Verification
According to the content of the sample in the sample solution, the selected concentration and sample solution similar to the standard working solution. Standard working solution and sample solution
The ketene response value should be within the linear range of the instrument. The standard working solution and sample solution were measured by volume injection. In the above liquid phase color
The retention time of cyclohexene ketone was 2.83 min, 3.40 min, thiazolone 3.81 min,
Oxaliplatin 3.89 min, olefinic acid 4.05 min, lettuceone 4.08 min, trimethylbenzenone 4.17 min, cycloasproxone 4.83 min.
Cyclodextone Standards for Liquid Chromatography-Mass Spectrometry/Mass Spectrometry Multi-Reaction Monitoring Chromatograms are given in Appendix B, Figure B.1.
In the above liquid chromatography-mass spectrometry conditions, the retention time of the material to be measured in the sample is different from that of the standard working solution.
± 2.5%, and the relative ion abundance of the test substance in the sample is compared with the relative ion abundance of the standard working solution,
The allowable relative deviation does not exceed the range specified in Table 2, it can be determined that there is a corresponding analyte in the sample.
Table 2 The maximum allowable deviation of relative ion abundance when qualitative confirmation
Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10%
Allowable relative deviation ± 20% ± 25% ± 30% ± 50%
7.4 blank test
In addition to the sample, according to the above steps.
Time (min) formic acid aqueous solution (3.9),% acetonitrile,%
0.25 60 40
1.50 60 40
1.60 40 60
2.00 40 60
3.00 20 80
4.50 20 80
5.00 60 40
6.00 60 40
8 results are calculated and expressed
Use the LC-MS/MS chromatographic data processor or calculate the residual content of cyclohexenyl ketone in the sample according to formula (1). The calculation result is deductible
value.
MΑsi
VCsiAi
(1)
Where.
Xi - The amount of cyclohexene ketone in the sample, in micrograms per kilogram (μg/kg);
The peak area of cyclohexene ketone in sample solution;
Csi - Concentration of cyclohexenyl ketone in standard working fluid in ng/ml (ng/mL);
V - the final volume of the sample solution in milliliters (mL);
Asi - the peak area of cyclohexene ketone in standard working fluid;
M - the mass of the 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 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 quantification limit of this method is 5 μg/kg.
10.2 Recovery rate
The data for the concentration, recovery and precision of the sample are given in Appendix C.
Appendix A
(Informative)
Mass spectrometry reference conditions
Table A.1 Mass Spectrometry Reference Conditions
Ion source ESI, positive mode
Scanning mode multiple reaction monitoring MRM
Source temperature 110 ℃
Solvent gas flow rate 550 L/hr, nitrogen
The solvent temperature was 350 ° C
Taper hole air flow 50 L/hr, nitrogen
Collision gas pressure 3.30 × 10 - 3 mbar, argon, purity ≥ 99.999%
Capillary voltage 3.0 KV
Table A.2 Multi-reaction monitoring conditions
Compound parent ion
(M/z)
Ion
(M/z)
Dwell time
(S)
Cone hole voltage
(V)
Collision energy
(EV)
Grass off
324.7 178.4
266.5 *
0.02 23 21
0.02 23 12
Thiadenone
326.4 180.2 0.02 20 20
280.3 * 0.02 20 13
Dilute pyridine
328.3 178.1 * 0.02 12 20
282.2 0.02 12 11
Trimethylbenzene
330.3 137.9 0.02 24 24
284.2 * 0.02 24 12
Pyranone
342.4 166.1 0.02 22 21
250.3 * 0.02 22 14
Oxadiazone 360.2 164.1 * 0.02 24 19
268.3 0.02 24 13
Butanone
400.4 138.1 0.02 28 23
354.3 * 0.02 28 15
Cyclohexanone
466.2 180.2 0.02 25 25
280.3 * 0.02 25 15
Note. The ions with "*" in Table A.2 are quantitative ions.
Non-commercial notices. The reference mass spectrometry conditions listed in Appendix A are performed on a Waters Quattro Premier LC/MS, where the test type
Is for reference only and does not involve commercial purposes and encourages standard users to attempt to use instruments of different manufacturers or models.
Appendix B
(Informative)
Cyclohexenone Standards Multi - Reaction Monitoring Chromatograms
Figure B.1 Cyclohexenone Standards Liquid Chromatography-Mass Spectrometry/Mass Spectrometry Multi-Reaction Monitoring Chromatogram
Appendix C
(Informative)
Recovery and precision
Table C.1 Data on the concentration, recovery and precision of the sample
(%) Concentration (%) Concentration of sample compound concentration (μg/kg) Recovery range (%) Precision (%) Concentration (%) Concentration (%) Concentration (%) Concentration (%
Pyranone 5 75.20 to 101.00 10.16
Pyrione 4 76.40 ~ 98.40 8.58
10 81.30 ~ 103.80 8.93 10 79.50 ~ 103.50 9.03
50 77.04 ~ 102.64 9.72 50 80.80 ~ 102.84 8.91
Herbs off 5 76.80 ~ 101.00 9.95 Herbs off 5 80.80 ~ 103.20 8.29
10 75.60 ~ 101.10 8.24 10 78.90 ~ 102.60 7.77
50 80.52 ~ 101.40 7.59 50 78.26 ~ 102.36 9.49
Thiabendone 5 76.4 ~ 102.20 9.73 Thiadenone 5 76.20 ~ 98.40 6.54
10 81.70 ~ 107.00 9.16 10 81.00 ~ 104.30 9.35
50 79.40 ~ 102.20 8.20 50 86.32 ~ 103.36 5.84
Oxadiazone 5 76.4 to 105.00 10.15 oxadiazone 5 83.20 to 109.40 9.23
10 75.90 ~ 94.10 6.76 10 80.60 ~ 104.80 10.02
50 73.24 ~ 94.58 9.73 50 80.44 ~ 100.32 8.26
Dilute pyridine 5 84.00 ~ 103.60 6.19 diltthlor 5 82.60 ~ 104.80 7.77
10 88.20 ~ 103.20 5.14 10 75.30 ~ 98.10 7.22
50 82.06 ~ 104.34 8.30 50 82.70 ~ 104.26 8.20
Table C.1 (continued)
Butoxfen 5 83.12 ~ 105.60 6.19
Butanone 5 77.40 to 103.20 10.02
10 80.00 ~ 98.40 5.14 10 76.90 ~ 97.30 8.31
50 79.46 ~ 100.62 8.30 50 77.42 ~ 102.86 10.22
Trimesterone 5 78.60 ~ 102.20 8.20 Trimethoproxone 5 76.20 ~ 107.00 7.90
10 81.20 ~ 104.20 7.84 10 80.50 to 101.70 10.39
50 87.12 ~ 103.76 5.94 50 80.86 ~ 99.56 6.14
Cyclohexanone
5 82.20 to 104.20 8.47
Cyclohexanone
5 81.60 ~ 108.60 8.58
10 74.20 ~ 101.00 8.24 10 77.60 ~ 98.70 5.89
50 78.76 ~ 94.84 6.45 50 78.94 ~ 98.34 8.31
Pyrrione 5 74.60 ~ 103.80 9.82
Pyrrione 5 78.40 ~ 99.60 7.97
10 79.10 ~ 97.30 6.58 10 78.10 ~ 102.10 11.19
50 75.80 ~ 98.76 7.93 50 83.12 ~ 100.64 7.69
Herbs off 5 76.80 ~ 101.40 7.12 Herbs off 5 73.60 ~ 98.40 5.67
10 81.50 to 101.10 6.53 10 78.40 to 100.70 7.61
50 77.66 ~ 96.88 7.43 50 80.22 ~ 99.34 8.32
Thiabendone 5 76.40 ~ 108.60 10.22 Thiomethoxone 5 76.40 ~ 101.20 6.33
10 78.90 ~ 101.70 9.00 10 76.70 ~ 101.30 9.71
50 78.28 ~ 102.12 8.96 50 83.36 ~ 104.20 7.91
Table C.1 (continued)
Oxadiazone 5 79.40 to 100.80 8.33
Oxadiazone 5 76.20 to 103.20 9.43
10 75.90 ~ 105.70 10.18 10 79.40 ~ 97.30 7.77
50 76.66 ~ 96.88 7.60 50 78.88 ~ 99.24 7.88
Dilute pyridine 5 77.20 ~ 103.60 8.87 diltthlor 5 75.80 ~ 106.40 10.24
10 76.40 ~ 104.70 10.47 10 78.50 ~ 103.50 9.25
50 79.52 ~ 101.46 7.74 50 78.86 ~ 97.00 6.68
Butroxydim ~ 5 74.40 99.40 76.00 5 8.34 butroxydim - 105.40 10.05
10 78.40 ~ 96.20 7.31 10 76.10 ~ 102.60 9.23
50 77.08 to 102.06 10.38 50 79.46 to 102.72 8.36
Trimethoproxone 5 74.20 to 103.40 9.66 Trimethylpenone 5 78.20 to 98.40 7.80
10 75.40 to 98.40 7.79 10 79.50 to 105.80 10.04
50 81.74 ~ 102.54 8.07 50 80.72 ~ 103.36 6.61
Cyclohexanone
5 77.40 ~ 103.80 9.48
Cyclohexanone
5 82.00 ~ 109.40 9.99
10 78.60 ~ 106.70 7.70 10 81.60 ~ 104.80 6.99
50 77.14 ~ 96.54 8.34 50 82.04 ~ 97.94 6.54
Pyrione 5 80.20 ~ 103.60 7.99 Spinach
Pyranone 5 81.20 to 106.80 8.60
10 79.40 to 103.20 9.10 10 78.90 to 101.60 8.33
50 84.12 ~ 102.84 6.79 50 80.22 ~ 99.24 7.57
Table C.1 (continued)
Grasses 5 77.40 ~ 103.60 8.87
Herbs off 5 80.40 ~ 104.80 9.47
10 79.50 to 103.30 8.75 10 76.20 to 103.50 9.12
50 82.90 ~ 104.62 7.50 50 8020 ~ 100.72 7.03
Thiadenone 5 82.20 ~ 105.40 8.45 Thiadenone 5 80.00 ~ 105.60 9.04
10 83.10 ~ 104.20 7.73 10 81.60 ~ 105.50 8.85
50 88.70 ~ 103.42 5.22 50 82.06 ~ 106.60 8.68
Oxadiazone 5 81.40 ~ 107.60 9.46 oxadiazone 5 82.60 ~ 100.00 7.17
10 81.60 ~ 105.40 8.16 10 84.00 ~ 105.70 7.59
50 84.70 ~ 101.94 6.71 50 83.20 ~ 108.06 6.88
Dilute pyridine 5 80.20 ~ 104.00 8.23 dilute pyridine 5 82.00 ~ 105.40 9.01
10 79.20 to 95.80 6.31 10 81.20 to 101.10 9.66
50 79.70 ~ 102.74 8.39 50 88.70 ~ 102.72 5.09
Butoxfen 5 77.60 ~ 105.60 10.55 Butanone 5 76.20 ~ 99.60 7.66
10 79.40 ~ 95.40 6.48 10 78.60 ~ 105.10 9.42
50 80.06 ~ 104.02 6.99 50 80.72 ~ 106.20 7.77
Trimesterone 5 83.20 to 108.20 8.14 Trimethoproxone 5 82.60 to 104.60 7.07
10 78.10 ~ 100.10 7.99 10 78.10 ~ 106.40 8.79
50 82.12 to 106.12 7.22 50 88.06 to 102.74 5.05
Table C.1 (continued)
Cyclohexanone
5 80.20 ~ 96.20 6.40 Spinach
Cyclohexanone
5 82.00 ~ 105.60 8.48
10 79.40 to 97.30 7.39 10 79.40 to 98.50 7.72
50 77.52 ~ 98.62 8.97 50 84.06 ~ 102.72 6.24
Pyrione 5 77.00 ~ 103.40 10.57
Pyrrione 5 73.20 ~ 104.80 11.33
10 81.00 ~ 104.10 7.61 10 79.50 ~ 103.50 9.13
50 77.04 ~ 100.62 8.70 50 84.06 ~ 102.84 7.51
Herbs off 5 77.80 ~ 98.00 8.08 Herbs off 5 80.80 ~ 105.40 8.84
10 78.50 to 98.40 8.39 10 79.10 to 102.60 8.52
50 78.86 to 102.14 9.61 50 84.08 to 102.50 6.00
Thiabendone 5 76.00 ~ 103.60 9.53 Thiomethoxone 5 80.20 ~ 98.40 6.88
10 81.00 ~ 99.70 6.80 10 79.40 ~ 105.80 9.80
50 79.46 ~ 106.72 8.59 50 84.12 ~ 103.36 5.83
Oxalcone 5 78.20 to 101.20 8.30 Elicenone 5 80.60 to 109.40 10.10
10 79.50 to 106.80 11.04 10 79.30 to 104.80 9.10
50 80.42 to 104.20 9.12 50 82.02 to 106.08 8.21
Diltiazem 5 80.20 ~ 105.20 8.12 dilute pyridine 5 81.80 ~ 102.40 8.65
10 79.40 ~ 100.40 7.58 10 79.80 ~ 98.70 6.74
50 75.68 ~ 104.72 9.74 50 78.22 ~ 98.52 7.13
Table C.1 (continued)
Butoxfen 5 76.62 ~ 102.80 9.85
Butoxfen 5 80.00 ~ 107.60 9.83
10 79.10 ~ 106.80 9.09 10 79.20 ~ 103.10 8.61
50 85.02 ~ 100.48 7.07 50 80.62 ~ 106.96 7.78
Trimesterone 5 80.60 ~ 101.60 8.25 Trimethoproxone 5 74.40 ~ 104.20 9.31
10 78.50 to 103.70 9.21 10 78.30 to 97.10 7.27
50 82.72 ~ 104.76 6.65 50 78.94 ~ 100.20 8.08
Cyclohexanone
5 81.20 ~ 103.60 9.63
Cyclohexanone
5 74.20 ~ 104.60 10.39
10 80.40 ~ 106.40 8.74 10 78.10 ~ 103.10 9.15
50 82.12 ~ 100.76 7.03 50 81.74 ~ 99.24 7.01
Pyrione 4 77.20 ~ 98.20 7.70
Pyrrione 5 74.60 ~ 97.20 6.30
10 80.10 ~ 103.90 9.76 10 78.90 ~ 98.40 6.88
50 82.12 ~ 102.68 7.43 50 78.96 ~ 98.62 8.49
Grasses 5 81.60 ~ 103.20 8.11 Grasses off 5 77.80 ~ 98.40 8.14
10 79.80 to 108.10 9.45 10 78.50 to 100.30 8.11
50 80.78 ~ 97.78 6.08 50 78.86 ~ 99.24 7.74
Thiabendone 5 81.20 to 99.60 6.60 Thiadenone 5 79.40 to 103.20 9.37
10 78.60 ~ 102.70 7.49 10 76.10 ~ 96.40 7.14
50 82.62 ~ 106.20 7.41 50 78.46 ~ 96.12 6.77
Table C.1 (continued)
Oxadiazone 5 83.20 to 104.60 7.61
Oxadiazone 5 81.20 to 104.80 9.26
10 78.10 ~ 106.40 8.80 10 79.60 ~ 100.10 8.05
50 80.06 to 99.24 6.98 50 80.60 to 100.12 7.59
Diltiazem 5 81.20 ~ 104.20 8.18 diltthlor 5 77.60 ~ 103.40 9.35
10 79.90 ~ 98.30 6.43 10 78.80 ~ 98.90 7.62
50 80.38 ~ 106.12 9.22 50 78.96 ~ 102.72 10.01
Butoxfen 5 74.80 to 107.20 11.15 Butoxfen 5 81.00 to 102.80 8.44
10 80.20 to 104.60 7.32 10 79.10 to 106.30 9.57
50 80.18 ~ 98.36 8.09 50 84.12 ~ 104.08 5.97
Trimesterone 5 77.20 to 105.40 9.29 Trimethoprostenone 5 77.40 to 103.20 8.18
10 78.40 ~ 106.70 9.75 10 79.50 ~ 103.70 9.17
50 76.92 ~ 99.24 8.32 50 82.72 ~ 102.84 7.86
Cyclohexanone
5 83.20 to 109.20 8.07
Cyclohexanone
5 76.40 ~ 105.40 10.17
10 79.50 to 103.00 8.93 10 83.10 to 106.40 8.60
50 76.98 ~ 99.76 9.13 50 82.12 ~ 100.10 6.59
Pyranone 5 83.80 to 100.20 6.53
Pyrrione 5 74.20 ~ 103.60 9.74
10 81.60 ~ 104.70 9.22 10 86.10 ~ 103.70 6.48
50 79.52 ~ 102.68 8.53 50 82.90 ~ 103.36 7.23
Table C.1 (continued)
Herbs off 5 74.40 ~ 103.20 9.40
Herbicide 5 85.20 ~ 109.40 9.02
10 81.20 to 108.10 8.99 10 79.50 to 104.20 8.09
50 78.94 ~ 98.48 6.74 50 84.26 ~ 106.08
Thiabendone 5 74.20 ~ 100.40 9.01 Thiadenone 5 82.20 ~ 100.00 5.97
10 78.60 ~ 98.40 7.79 10 79.80 ~ 98.70 6.37
50 83.16 ~ 106.20 7.27 50 82.06 ~ 99.04 9.02
Oxadiazone 5 77.40 ~ 104.60 10.34 oxadione 5 80.40 ~ 100.20 7.48
10 78.10 ~ 106.40 9.71 10 79.20 ~ 94.20 5.49
50 78.82 ~ 99.24 7.49 50 79.70 ~ 98.22 7.53
Diltiazem 5 82.00 ~ 104.80 9.25 dilute pyridine 5 78.40 ~ 100.60 8.40
10 79.60 ~ 96.20 5.68 10 82.60 ~ 105.20 7.69
50 81.94 ~ 99.34 5.95 50 79.02 ~ 97.52 6.55
Butenone 5 80.20 to 103.40 8.39 Butanone 5 81.40 to 104.80 8.50
10 79.10 ~ 95.60 6.29 10 78.10 ~ 102.60 9.74
50 79.70 ~ 99.30 7.61 50 80.44 ~ 107.76 7.94
Trimesterone 5 77.00 ~ 100.60 8.25 Trimethoproxone 5 83.20 ~ 106.80 8.70
10 79.40 ~ 96.70 7.01 10 80.30 ~ 101.20 10.70
50 82.06 ~ 99.24 7.09 50 80.72 ~ 98.04 7.64
Cyclohexanone
5 80.40 ~ 98.40 7.74
Cyclohexanone
5 82.00 ~ 106.00 9.41
10 78.10 ~ 103.50 9.17 10 81.60 ~ 102.60 9.27
50 82.12 ~ 98.74 6.85 50 80.12 ~ 98.50 6.71
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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