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GB 23200.69-2016: Food safety national standard -- Determination of Dinitroaniline Pesticide Residues in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry
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Food safety national standard -- Determination of Dinitroaniline Pesticide Residues in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry
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GB 23200.69-2016
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Basic data | Standard ID | GB 23200.69-2016 (GB23200.69-2016) | | Description (Translated English) | Food safety national standard -- Determination of Dinitroaniline Pesticide Residues in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 15,114 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 2795-2011 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.69-2016: Food safety national standard -- Determination of Dinitroaniline Pesticide Residues in Food by Liquid Chromatography -- Mass Spectrometry / Mass Spectrometry
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Food safety national standard - Determination of Dinitroaniline Pesticide Residues in Food by Liquid Chromatography - Mass Spectrometry/Mass Spectrometry
National Standards of People's Republic of China
GB
Instead of SN/T 2795-2011
National standards for food safety
Determination of Dinitroaniline Pesticide Residues in Food
Liquid chromatography - mass spectrometry/mass spectrometry
National food safety standards-
Determination of dinitroaniline pesticides residue 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 2795-2011 "Determination of Dinitroaniline Pesticide Residues in Import and Export Foods Liquid Chromatography-Mass Spectrometry/Tandem
Mass spectrometry ".
Compared with SN/T 2795-2011, 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 "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 2795-2011.
National standards for food safety
Determination of Dinitroaniline Pesticide Residues in Food
Liquid chromatography - mass spectrometry/mass spectrometry
1 Scope
This standard specifies the method for the determination of eight dinitroaniline pesticide residues in food by liquid chromatography-mass spectrometry/mass spectrometry.
This standard applies to soybeans, rice, spinach, ginger, apple, watermelon, cabbage, saucer, tea, eggs, pork and chicken liver fluoride
Lentin, Pendimethalin, Ammonolate, Sulfamethoxazole, Ammonolol, Ammonol, Methrone and Isoleveline, etc. Dinitroanilide Pesticide Residues
The determination and confirmation of the amount of food; other food can refer to the implementation.
2 normative reference documents
The documentation is essential for the application of this document. For dated references, only the dated edition applies to this document.
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, extracted with graphitized carbon black solid phase extraction column and HLB solid phase extraction column. The liquid chromatography-tandem mass spectrometry
Fixed and confirmed, 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 Methanol (CH3OH). Chromatographic Purification.
4.1.2 acetonitrile (CH3CN). pure chromatography.
4.1.3 n-hexane (C6H14). chromatographic purity.
4.1.4 Formic acid (CH2O2). Chromatographic purity.
4.1.5 Acetone (C3H6O). excellent grade pure.
4.1.6 Sodium chloride (Nacl). Analytical purity.
4.1.7 anhydrous sodium sulfate (Na2SO4). analytical grade, with 650 ℃ before burning 4 h, set the dryer in the spare.
4.2 solution preparation
4.2.1 acetonitrile-water solution (1 1, containing 0.05% formic acid). 500 mL of acetonitrile and 0.5 mL of formic acid in 1 L volumetric flask,
Set to 1 L, mix well.
4.2.2 n-hexane - acetone solution (2 8). take 20 mL of n-hexane, add 80 mL of acetone, mix.
4.3 standards
4.3.1 Dinitroaniline Pesticide Reference Material. See Appendix A, Table A.1.
4.4 standard solution preparation
4.4.1 dinitroaniline pesticide standard stock solution. accurately weighed appropriate amount of dinitroaniline pesticide standard substances, with acetone with
A standard stock solution at a concentration of 1000 mg/L was prepared and the standard solution was kept at -18 ° C for a period of 12 months.
4.4.2 dinitroaniline pesticide mixed intermediate standard solution. absorb the appropriate amount of the standard stock solution, diluted with methanol into the concentration of trifluralin
For the 5.0mg/L, the other seven kinds of drug concentration of 1.0 mg/L mixed intermediate standard solution, 0 ℃ ~ 4 ℃ dark preservation, shelf life of 3 months.
4.4.3 matrix mixed standard working solution. absorb the appropriate amount of mixed intermediate standard solution, with blank sample extract with fen lering concentration
0μg/L, 50μg/L, 100μg/L, 250μg/L, 500μg/L and 1000μg/L, the other seven pesticide concentrations were 0μg/L, 10.0μg /
20.0 μg/L, 50.0 μg/L, 100 μg/L and.200 μg/L, respectively. The day of preparation.
4.5 Materials
4.5.1 Graphitized Carbon Black Solid Phase Extraction Column. 3 mL 250 mg, or equivalent. Activate the column with the first 3 mL n-hexane-acetone solution
Moist.
4.5.2 Oasis HLB1, 6mL,.200mg, or equivalent. Activate with 5 mL acetonitrile before use to keep the column moist.
5 instruments and equipment
5.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer. Equipped with an electrospray ion source (ESI).
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 Crusher.
5.4 Tissue crusher.
5.5 Scroll Mixer.
5.6 Solid phase extraction unit with vacuum pump.
5.7 nitrogen blowing concentrator.
5.8 Centrifuge. speed of not less than 5 000 r/min.
6 Preparation and storage of samples
6.1 Preparation of the sample
6.1.1 soybeans, tea and rice
Approximately 500 g of the sample was taken (not with water). After shredding, the sample was processed into a slurry by a crusher and mixed. The samples are divided into
Two, into a clean container, sealed, and marked with a mark.
6.1.2 vegetables, fruits, eggs, pork and chicken liver
Approximately 500 g of the sample was taken (not with water). After shredding, the sample was processed into a slurry by a crusher and mixed. The samples are divided into
Two, into a clean container, sealed, and marked with a mark.
Note. The above sample sampling site according to GB 2763 Appendix A implementation.
6.2 Sample storage
During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue. Soybeans, tea and rice samples in the often
Save under temperature. Vegetables, fruits, eggs, pork and chicken liver samples are stored at -18 C.
7 Analysis steps
7.1 Extraction
7.1.1 soybeans, rice, tea, eggs, pork and chicken liver
For tea, soybeans, chestnuts, and corn samples, weigh 2.5 g of the sample (accurate to 0.01 g). For spinach, mushrooms, apples, cow
Meat, beef, chicken, fish, milk samples, weighed 5 g sample (accurate to 0.01 g). The weighed sample was placed in a 50 mL centrifuge tube,
Add 6 mL of saturated aqueous sodium chloride solution and mix for 30 s on a vortex mixer for 15 min. Add 6 mL of acetone to n-hexane solution
Mix the mixers for 2 min. 5 000 r/min centrifugation 1 min, the upper layer of extract in another test tube. And then add 4 mL of acetone - plus
The alkane solution was repeatedly extracted twice and the combined extracts were purged with nitrogen at about 45 ° C to about 1 mL to be purified.
7.1.2 Vegetables, fruits
Weigh about 5 g (exactly to 0.01 g) of the sample in a 50 mL stoppered centrifuge tube, then add 2 g of sodium chloride, add 15 mL of acetonitrile
The homogeneity was extracted for 3 min and centrifuged at 5 000 r/min for 5 min. The acetonitrile layer was transferred to a 25 mL volumetric flask. The residue was repeated with 10 mL of acetonitrile
Extract once, combine the extract and freeze to 25 mL with acetonitrile.
7.2 Purification
7.2.1 soybeans, rice, pork
The whole concentrated extract was aspirated in a Supelclean C18 solid phase extraction column at a flow rate of about 1.5 mL/min.
The column was extracted and washed with 5 mL of acetonitrile and the solid phase extraction was dried. The whole effluent was collected in a 1.5 mL centrifuge tube and treated with nitrogen
Air blowing to near dry, the residue with acetonitrile aqueous solution to 1.0 mL. After vortexing, the microporous membrane was passed through a liquid chromatography-mass spectrometer/mass spectrometer
Determination.
7.2.2 vegetables, fruits
Accurate draw 5 mL extract 5.0 mL in 15 mL centrifuge tube, below 40 ℃ with nitrogen blowing to near dry, with 2.0 mL n-hexane -
Acetone solution was dissolved and transferred to an Envi-carb solid phase extraction column. The solution was passed through a solid phase extraction column at a flow rate of about 1.5 mL/min.
Non-commercial statement. Column models are listed here for reference only and are not intended for commercial purposes. Encourage standard users to attempt to use different manufacturers or specifications
Of the column.
The solid phase extraction column was rinsed with 3 mL of n-hexane-acetone solution and the whole effluent was collected in a 15 mL centrifuge tube.
Air blowing to near dry, the residue with acetonitrile aqueous solution to 1.0 mL. After mixing the vortex, the microporous membrane was measured by liquid chromatography-mass spectrometry/mass spectrometer
set.
7.2.3 Tea, eggs and chicken liver
Extraction of tea, eggs and chicken liver concentrated extract in the Oasis HLB solid phase extraction column, the flow rate of about 1.5 mL/min
The solid phase extraction column was washed with 5 mL of acetonitrile and the solid phase extraction column was drained. The whole effluent was collected in a 15 mL centrifuge tube at 40 ° C
Was purged with nitrogen to near dryness, dissolved in 2.0 mL n-hexane-acetone solution, transferred to Envi-carb solid phase extraction column at about 1.5 mL/min
The flow rate was passed through a solid phase extraction column and eluted with 3 mL of n-hexane-acetone solution and the solid phase extraction column was drained.
Liquid in 15 mL centrifuge tube, below 40 ℃ with nitrogen blowing to near dry, the residue with acetonitrile aqueous solution to 1.0 mL. After mixing the vortex,
Microporous membrane for liquid chromatography - mass spectrometry/mass spectrometry.
7.3 Determination
7.3.1 Liquid Chromatographic Reference Conditions
A) Column. C18 column, 50 mm × 2.1 mm (id), 1.7 d., Or equivalent;
B) Column temperature. 40 ° C;
C) Injection volume. 10 μL;
D) The mobile phase, flow rate and gradient elution conditions are shown in Table 1.
Table 1 Mobile phase, flow rate and gradient elution conditions
time
Min
Flow rate
ML/min
0.05% formic acid - 5 mM acetate - aqueous solution
Methanol
0 0.30 50 50
5.0 0.30 20 80
8.0 0.30 0 100
9.5 0.30 50 50
7.3.2 Mass spectrometry reference conditions
A) ionization mode. electrospray ion source;
B) Scanning mode. positive ion scanning;
C) Detection method. Multiple reaction monitoring (MRM);
D) Resolution. Unit resolution;
See Appendix B for other reference mass spectrometry conditions.
7.3.3 Qualitative determination
Each selected component selected one parent ion, two or more child ions, in the same experimental conditions, the sample retention time of the material to be tested,
And the substrate standard solution retention time deviation within ± 2.5%; and the sample of each component of the relative abundance of ions and concentrations close to the matrix
Comparing the relative abundance of the corresponding qualitative ions in the standard working solution, the deviation does not exceed the range specified in Table 2,
There is a corresponding test substance in the product.
Table 2 shows the maximum allowable error for relative ion abundance when qualitatively by liquid chromatography-tandem mass spectrometry
Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10%
Allowable relative deviation ± 20% ± 25% ± 30% ± 50%
7.3.4 Quantitative determination
The best working conditions of the instrument, the substrate mixed with the standard working solution into the peak area for the vertical axis, the matrix mixed standard working solution
Concentration for the abscissa to draw the standard working curve, with the standard working curve of the sample quantitative. The response value of the analyte in the sample solution should be
In the linear range of the assay method, if the linear response range is exceeded, the blank matrix solution is used for proper dilution. In the above liquid chromatography-
The retention times of dinitroaniline pesticides were. salbutam (3.21 min), methotrexate (3.41 min)
Ammonofural (4.06 min), Ammonolone (5.20 min), Pentylenol (5.36 min), Zhong Dingling (5.70 min), trifluralin (5.70 min)
Min and isoproterenol (6.06 min). The chromatogram of mass spectrometry for mass spectrometry/mass spectrometry/mass spectrometry is shown in Figure C.1 in Appendix C.
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 dinitroaniline pesticide in the sample according to the following formula (1).
MΑsi
VCsiAi
.. (1)
Where.
X - Residual content of each dinitroaniline pesticide in the sample, in milligrams per kilogram, mg/kg;
The peak area of each dinitroaniline pesticide in the sample solution;
V - the final volume of the sample solution, in milliliters, mL;
Asi - the peak area of each dinitroaniline pesticide in standard working fluid;
Csi - Concentration of each dinitroaniline pesticide in standard working fluid 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 reproducible conditions and their arithmetic mean (percentage) shall be in accordance with the
Record the requirements of E.
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 the
Record F requirements.
10% limit and recovery rate
10.1 Quantitation limits
The limit of quantification of dinitroaniline pesticides is 0.01 mg/kg.
10.2 Recovery rate
When adding levels of 0.05 mg/kg, 0.1 mg/kg, 0.2 mg/kg, the recovery of dinitroaniline pesticides is given in Appendix D.
Appendix A
(Informative)
Dinitroaniline pesticide
Table A.1 Related information about dinitroaniline pesticides
Compound name English name Cas No. molecular formula molecular weight molecular structure
Trifluralin 1582-09-8 C13H16F3N3O4 335.28
Pendimethalin 40487-42-1 C13H19N3O4 281.31
Zhong Dingling Butralin 33629-47-9 C14H21N3O4 295.33
Isopropalin 33820-53-0 C15H23N3O4 309.36
Amoxicillin Dinitramine 29091-05-2 C11H13F3N4O4 322.24
Nitrone Nitrone
Amoxicillin Oryzalin 19044-88-3 C12H18N4O6S 346.36
Ampicillin Prodiamine 29091-21-2 C13H17F3N4O4 350.29
Appendix B
(Informative)
Mass spectrometry conditions
A) electrospray voltage. 3000 V;
B) Auxiliary gas flow rate. 750 L/h;
C) collision gas. argon;
D) curtain air flow rate. 50 L/h;
E) ion source temperature. 105
F) Auxiliary gas temperature. 350 auxiliary;
G) Qualitative ion pair, quantitative ion pair, acquisition time, cone hole voltage and collision energy are shown in Table B.1.
Table B.1 Mass Spectrometric Parameters of Dinitroaniline Pesticide Reference Material
Analyte
Reference retention time
Min
Mother ion
(M/z)
Ion
(M/z)
Acquisition time
Cone hole voltage
Collision energy
EV
Trifluralin 5.70 336.2
236 * 0.1
252 0.1 23
Pendimethalin 5.36 282
212 * 0.05
194 0.05 17
Zhong Dingling 5.70 296
240 * 0.05
222 0.05 20
Isopropyl Lose 6.06 310
226 * 0.05
268 0.05 14
Ampicillin 4.06 323
289 * 0.05
247 0.05 16
Methasone Lentin 3.41 346
304 * 0.05
262 0.05 22
Amoxicillin 3.21 347
288 * 0.05
305 0.05 14
Ammonofluramine 5.20 351
267 * 0.05
291 0.05 18
Note. * for the quantitative ions, for different mass spectrometry equipment, instrument parameters may be different, should be measured before the mass spectrometry parameters to optimize the best.
Non-commercial declaration. The reference mass spectrometry conditions listed in B.1 are performed on a Waters Quattro Premier LC/MS, where the test instrument model
Only for reference, does not involve commercial purposes, to encourage standard users to try different manufacturers or models of equipment.
Appendix C
(Informative)
Standard Quality Spectrum of 8 Dinitroaniline Pesticides
Figure C.1 Standard spectra of eight dinitroaniline pesticides
Appendix D
(Informative)
The recoveries of dinitroanilines in different matrices
Table D.1 Recovery of dinitroanilines in different matrices
Compounds
name
Add water
Μg/kg
Rice recovery rate
range
Recovery rate of soybeans
range
Apple recovery rate
range
Watermelon Recycling
range
Recovery of melon
range
Ginger recycling
range
Spinach recycling
range
Cabbage recycling
range
Tea recycling
range
Egg recycling
range
Pork recycling
range
Chicken liver recovery
range
Trifluralin
50.0 74.7 to 98.8 103 to 116 74.9 to 115 93.3 to 120 79.8 to 98.6 87.3 to 111 72.6 to 82.4 72.5 to 78.4 75.8 to 99.6 100 to 112 71.2 to 75.5 73.1 to 79.1
100 77.1 to 114 89.2 to 119 71.8 to 88.6 79.7 to 102 85.0 to 112 76.3 to 109 71.5 to 92.6 70.5 to 81.5 77.3 to 96.5 99.9 to 111 70.2 to 73.0 70.6 to 77.8
200 76.0 to 115 70.8 to 122 75.1 to 98.9 76.4 to 103 72.4 to 97.4 70.2 to 81.1 70.5 to 86.0 71.5 to 76.8 77.5 to 84.0 74.0 to 85.5 71.5 to 77.3 74.6 to 80.5
Paclitaxel
10.0 88.0 to 118 79.0 to 95.0 95.1 to 121 70.6 to 73.7 74.6 to 118 86.2 to 116 79.0 to 95.0 89.4 to 98.2 71.0 to 79.0 89.0 to 96.0 73.5 to 87.3 85.3 to 96.9
50.0 77.7 to 105 84.6 to 99.6 82.4 to 110 70.5 to 103 83.0 to 114 86.3 to 97.8 84.6 to 95.0 85.9 to 96.8 71.2 to 77.8 81.8 to 91.8 80.2 to 95.9 80.7 to 91.0
200 85.0 to 119 73.5 to 96.0 89.1 to 118 73.8 to 82.0 76.0 to 94.2 83.9 to 101 73.5 to 96.0 91.2 to 96.9 85.5 to 89.0
74.5 ~ 82.5 84.5 ~ 98.5 70.4 ~ 78.8
Ammonolate
10.0 91.0 to 115 80.4 to 96.8 99.1 to 121 72.5 to 115 97.9 to 119 84.7 to 107 83.0 to 101 92.6 to 94.1 80.0 to 99.0 87.6 to 94.2 75.3 to 96.7 83.6 to 98.7
50.0
79.0 to 115 91.0 to 117 91.4 to 108 83.7 to 100 95.1 to 116 79.1 to 104 84.4 to 109 91.7 to 98.4 74.2 to 79.4 78.3 to 83.3 82.9 to 96.4 83.7 to 97.8
100 79.5 to 120 71.0 to 115 90.9 to 121 85.8 to 94.0 88.3 to 108 70.6 to 92.0 84.4 to 109 91.7 to 98.8 72.8 to 88.8 93.0 to 99.0 85.3 to 99.0 91.6 to 95.9
Zhong Dingling
10.0 91.0 to 118 70.7 to 98.0 103 to 113 70.6 to 76.2 95.6 to 120 91.5 to 98.7 75.0 to 98.0 91.9 to 95.7 71.0 to 78.0 81.0 to 94.0 70.6 to 91.5 77.2 to 95.6
20.0
72.5 to 104 74.5 to 94.0 87.5 to 101 70.6 to 87.8 91.7 to 106 86.5 to 96.8 74.5 to 94.0 91.8 to 95.5 92.0 to 105 75.5 to 83.6 83.9 to 98.5 79.9 to 97.9
50.0 81.4 to 119 74.8 to 89.8 85.8 to 116 70.8 to 72.8 87.6 to 99.8 79.6 to 88.3 74.8 to 89.8 91.8 to 94.1 98.0 to 101 84.0 to 95.0 86.9 to 97.9 87.5 to 98.4
Isoprofen
10.0 86.0 to 119 76.0 to 83.0 96.6 to 122 70.0 to 75.1 96.1 to 122 71.7 to 81.2 76.0 to 83.0 91.5 to 98.5 70.0 to 81.0 81.5 to 94.0 70.6 to 90.2 76.2 to 93.2
20.0
78.5 to 107 77.5 to 89.5 85.6 to 97.7 72.2 to 89.8 85.3 to 106 75.7 to 83.0 79.0 to 94.0 90.9 to 98.8 87.5 to 100 74.2 to 78.0 81.4 to 89.3 78.1 to 91.4
50.0 70.8 to 120 73.0 to 89.0 76.8 to 104 70.9 to 79.9 71.3 to 95.1 70.5 to 75.0 71.0 to 89.0 91.2 to 95.7 86.1 to 95.7 74.2 to 78.0 82.6 to 90.5 83.1 to 91.6
Ammonofen 10.0 88.0 to 120 71.0 to 89.0 102 to 116 72.1 to 82.0 96.4 to 115 78.4 to 95.6 79.0 to 91.5 89.1 to 97.4 70.0 to 81.0 94.0 to 102 72.1 to 98.9 71.8 to 92.3
20.0
76.5 to 119 82.1 to 104 90.5 to 111 70.5 to 91.8 97.0 to 118 78.4 to 90.8 79.0 to 91.4 91.3 to 99.0 87.5 to 100 83.5 to 92.5 89.9 to 98.8 84.8 to 96.7
50.0 83.8 to 119 79.0 to 91.5 93.4 to 110 71.3 to 86.8 86.7 to 107 78.3 to 92.5 70.0 to 95.4 90.8 to 96.1 78.8 to 88.6 80.2 to 109 92.0 to 98.8 90.8 to 98.7
Methrone
10.0 91.0 to 112 70.0 to 95.4 95.3 to 120 76.9 to 118 98.1 to 125 88.9 to 111 74.4 to 94.0 91.9 to 97.2 86.0 to 99.0 100 to 109 74.2 to 92.5 77.8 to 97.7
20.0
70.7 to 105 74.0 to 94.0 92.7 to 104 91.1 to 98.2 96.5 to 118 84.9 to 103 84.0 to 96.8 90.7 to 97.4 91.0 to 110 83.0 to 103 91.3 to 98.6 91.7 to 95.1
50.0 83.2 to 115 84.0 to 97.5 94.2 to 112 83.4 to 96.6 97.7 to 118 81.4 to 92.4 83.0 to 96.8 91.2 to 93.6 82.5 to 91.5 88.0 to 95.0 92.1 to 97.3 91.7 to 97.6
Amaranth
10.0 77.5 to 101 79.5 to 112 93.5 to 123 71.1 to 91.5 77.9 to 119 88.2 to 107 72.0 to 89.0 91.9 to 92.9 70.0 to 80.0 81.5 to 97.0 91.9 to 96.2 85.1 to 99.4
20.0
75.5 to 114 71.0 to 99.5 82.2 to 106 71.9 to 84.7 95.5 to 106 87.9 to 106 71.0 to 99.5 90.8 to 92.6 91.5 to 96.5 81.2 to 83.6 82.9 to 96.4 80.1 to 98.1
50.0 74.8 to 113 80.4 to 100 83.1 to 108 71.9 to 81.4 85.3 to 105 80.0 to 87.2 80.4 to 100 88.3 to 96.3 94.5 to 105 80.2 to 101 87.3 to 96.6 76.1 to 87.1
Appendix E
(Normative appendix)
Laboratory repeatability requirements
Table E.1 Laboratory repeatability requirements
Measured component content
Mg/kg
Precision
0.001 36
> 0.01
> 1 14
Appendix F
(Normative appendix)
Inter-laboratory reproducibility requirements
Table F.1 Inter-laboratory reproducibility requirements
Measured component content
Mg/kg
Precision
0.001 54
> 0.01
> 1 19
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