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Food safety national standard -- Detection Method of 9 Kinds of Organic Heterocyclic Pesticide Residues in Tea
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GB 23200.26-2016
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Basic data | Standard ID | GB 23200.26-2016 (GB23200.26-2016) | | Description (Translated English) | Food safety national standard -- Detection Method of 9 Kinds of Organic Heterocyclic Pesticide Residues in Tea | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 11,129 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 1591-2005 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.26-2016: Food safety national standard -- Detection Method of 9 Kinds of Organic Heterocyclic Pesticide Residues in Tea ---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 - Detection Method of 9 Kinds of Organic Heterocyclic Pesticide Residues in Tea
National standards for food safety
Three kinds of organic heterocyclic pesticide residues in tea
Detection method
National food safety standards-
Determination of 9 organic heterocyclic pestcides residues in tea
GB
National Standards of People's Republic of China
Instead of SN/T 1591-2005
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 1591-2005 "Method for the detection of nine kinds of organic heterocyclic pesticide residues in tea leaves".
This standard and SN/T 1591-2005, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- Standard name "import and export tea" to "tea".
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 1591-2005.
National standards for food safety
Detection Method of 9 Kinds of Organic Heterocyclic Pesticide Residues in Tea
1 Scope
This standard specifies the sampling and preparation of 9 kinds of organic heterocyclic pesticide residues in tea, the determination method, the determination of low
Limit and recovery rate.
This standard applies to tea in atrazine, vinblastin, pyrithione, fluconazole, imazalazole, buprofezin, propiconazole,
Chlorophenoxyprins, pyridaben residues in the test, other food can refer to the implementation.
2 normative reference documents
The following documents are indispensable for the application of this document. Note the date of the reference file, only the date of the date
Apply 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 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.
3.1 Reagents
3.1.1 Acetone (CH3COCH3). Distillation.
3.1.2 n-hexane (C6H14). re-distillation.
3.1.3 Sodium chloride (NaCl).
3.2 solution preparation
3.2.1 Acetone-n-Hexane (1 3) Solution. Take 100 mL of acetone, add 300 mL of n-hexane and shake well.
3.2.2 Acetone - n-Hexane (2 1) Solution. Take.200 mL of acetone, add 100 mL of n-hexane and shake well.
3.3 standards
3.3.1 Pesticide standards. purity ≥ 99%.
3.4 standard solution preparation
3.4.1 standard solution. accurately weighed amount of atrazine, vinblastin, pyrithione, fluconazole, imazalazole, buprofezin,
Propiconazole, chlorophenyl pyrimidol, pyridaben standard, with acetone prepared into a concentration of 1.00 mg/mL standard stock solution. And then according to
Need to use n-hexane diluted to the corresponding standard working fluid.
3.5 material
3.5.1 anhydrous sodium sulfate (Na2SO4). after 650 ℃ burning 4h, placed in the dryer in reserve.
3.5.2 Activated Carbon Solid Phase Extraction Column. 250 mg or equivalent.
3.5.3 Neutral alumina solid phase extraction cartridge. 250mg or equivalent.
4 instruments and equipment
4.1 Gas chromatograph with mass selective detector.
4.2 Analysis of balance. 0.01 g and 0.0001 g.
4.3 solid phase extraction device with vacuum pump.
4.4 multi-function micro-sample processor, or equivalent.
4.5 Centrifuge. 4 000r/min.
4.6 Scroll Mixer.
4.7 Centrifuge tube. 15mL.
4.8 scale tube. 15mL.
4.9 microinjector. 10 μL.
5 Preparation and storage of samples
5.1 Preparation of the sample
The recovered sample is ground and the sampling site is carried out according to GB 2763 Appendix A, passing through a 0.84 mm
Uniform, are divided into two, into a clean container, as a sample. Sealed and marked with mark.
5.2 Sample storage
Keep the sample below 5 ° C in dark. During sampling and sample preparation, it is necessary to prevent contamination of the sample
The change in residue content occurs.
6 Analysis steps
The presence of residual atrazine, vinblastide, pyrithione, fluconazole, imidazole, buprofezin, propiconazole, chlorine
Pyrimethanol, pyridaben is extracted with acetone-n-hexane, purified by activated charcoal column and neutral alumina column.
Acetone-n-hexane elution. After purification with gas chromatography, with mass spectrometry detector determination, external standard quantitative.
6.1 Extraction
Accurately weigh 1 g homogeneous sample (accurate to 0.001g) in a 15 ml centrifuge tube, add 1 g of sodium chloride, add 2 mL of steam
Water, mix on the mixer for 30 s, place it for 30 min, add 4 mL of acetone and n-hexane mixture, mix well on the mixer
2 min. Centrifuge at 2 500 r/min for 1 min and draw the upper n-hexane extract in another 15 mL graduated tube. And then points
Do not add 2 mL of acetone and n-hexane mixture to extract twice, the combined extract, add 1 g anhydrous sodium sulfate to dry. will
The dried extract was completely transferred to another clean scale tube placed on a microtiter sample processor at 50 ° C,
To about 1 mL (solution A).
6.2 purification
The activated carbon solid phase extraction column and neutral alumina solid phase extraction column (activated carbon solid phase extraction column filled about 1cm high
Of the anhydrous sodium sulfate layer) from top to bottom installed in the solid-phase extraction of the vacuum filter device, first with 1 mL × 3 acetone pre-leaching small
Column, and then 1 mL x 3 n-hexane pre-leaching column, keep the drip rate of 0.5 mL/min, discard all eluent.
The solution A was subjected to a solid-phase extraction solid column and a neutral alumina solid phase extraction column, followed by 6.0 mL of acetone and
The mixture was eluted and the whole eluent was collected and placed at 50 ° C and the nitrogen stream was blown to near dryness. Finally, with n-hexane
0.5 mL for GC-MSD analysis.
6.3 Determination
6.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions
A) Column. quartz capillary column, 5% phenylmethylpolysiloxane stationary phase. 30 m x 0.20 mm (inner diameter), film thickness
0.25μm, or equivalent;
B) Column temperature. 70 ° C for 2 min, rise to 180 ° C at 8 ° C/min, rise to 280 ° C at 3 ° C/min,
Keep for 18 min;
C) Inlet temperature. 250 ° C;
D) chromatographic - mass spectrometer interface temperature. 220 ° C;
E) Carrier gas. helium (purity > 99.995%), 0.6 mL/min;
F) Injection volume. 1 μL;
G) Injection method. no split injection, 1 min after the opening valve;
H) ionization mode. EI;
I) ionization energy. 70 ev;
J) Measurement method. Select the ion monitoring mode (SIM);
K) monitoring ions (m/z). see Table 2;
I) solvent delay. 15 min.
Table 2 9 Monitoring of heterocyclic pesticides in ions
Pesticide collection time/min Monitoring ions (m/z)
Atrazine 15 to 20 173, 187,.200a), 215
Vibrio Bacteria 20 ~ 25 187,198,212 a), 285
Pythium 25 ~ 26.5 96a), 255,283,285
Fenfluazole 25 to 26.5 219, 248, 278a), 287
Oxytocin 26.5 to 28.2 173 a), 215, 240, 296
Buprofezin 28.2 ~ 30.5 105a), 172,175,305
Propiconazole 30.5 to 36 173a) .191.259.261
Chlorophenyl pyruvate 36-40.5 139a), 219,251,330
Pyridenopsis 40.5 ~ 43 117,147a), 309,364
A)
The labeled ions are quantitative ions
6.3.2 Chromatographic determination
According to the sample in the atrazine, vinblastide, pyrithione, fluconazole, imazalazole, buprofezin, propiconazole, chlorobenzene
Pyrimethanol, pyridaben content of the situation, selected peak area similar to the standard working solution. Standard working solution and sample solution
Thiocarbamate, pyrithione, chlorpheniramine, imidazole, buprofezin, propiconazole, chlorophenyl pyruvate,
The values shall be within the linear range of the instrument detection. The sample solution of the standard working fluid was measured by volume injection. In the above chromatogram
Conditions, the standard SIM chromatogram is shown in Appendix A, Figure A.1.
6.3.3 Confirmation of mass spectrometry
The standard solution and sample solution were determined according to the conditions specified in 4.4.3.1, if the same solution in the sample solution with the standard
Leaving time there is a peak, then its mass spectrometry confirmed. When the relative abundance of the monitored ions is consistent with the standard,
And the similarity is plus or minus 10%, can confirm the test object. Under the above gas chromatographic - mass spectrometric conditions, nine heterocyclic pesticides
The retention time and the monitoring ion abundance ratio (m/z) are shown in Table 3.
Table 3 9 kinds of heterocyclic pesticide retention time and monitoring of ion abundance ratio
Pesticide retention time/min Monitoring ion abundance ratio
Atrazine 18.41 173. 187..200. 215 (26. 3. 100. 58)
Velvetlein 21.09 187. 198. 212. 285 (74. 89. 100. 86)
Phytophthora 25.46 96. 255. 283. 285 (100. 8. 69. 5)
Fluorobenzene 25.67 219. 248. 278. 287 (18. 7. 100. 53)
Antimoxazole 27.33 173. 215. 240. 296 (76. 100. 9. 6)
Buprofezin 28.30 105. 172. 175. 305 (100. 35. 25. 6)
Propiconazole 32.20,32.58 173. 191. 259. 261 (100. 27. 88. 57)
Chlorophenylpyrimidol 39.12 139. 219. 251. 330 (100. 63. 54. 36)
Pyridinone 41.64 117. 147. 309. 364 (15. 100. 7. 6)
6.4 blank experiment
In addition to the sample, according to the above determination steps.
7 Results calculation and presentation
Determination of atrazine, vinorelbine, pyrithione, fenfluazole in the sample by chromatographic data processor or by formula (1)
Miconazole, Myclobutanil, Buprofezin, Propiconazole, Chlorophenylpyrimidinol, Pyridinone Content.
VA
(1)
Where.
X-samples of atrazine, vinblastomycin, pyrithione, fluconazole, imidazole, nitrobenzazole, buprofezin, propiconazole,
The content of chlorpheniramine and pyridaben in milligrams per kilogram (mg/kg);
A sample of atrazine, vinblastin, pyrithione, fluconazole, imazalazole, nitrobenzazole, buprofezin, propiconazole,
The peak area of the plant is the square millimeter (mm2);
Cs-standard working solution of atrazine, vinblastin, pyrithione, fluconazole, imidazole, nitrobenzazole, buprofezin,
The concentration of propiconazole, chlorpheniramine and pyridaben in micrograms per milliliter (μg/mL);
As-standard working solution of atrazine, vinblastin, pyrithione, fluconazole, imidazole, nitrobenzazole, buprofezin,
The peak area of propiconazole, chlorpheniramine, pyridaben, in square millimeters (mm2);
The final volume of V-sample solution in milligrams (mL);
M - the amount of sample represented by the final sample, in grams (ɡ).
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.
8 precision
8.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage)
Rate), shall comply with the requirements of Appendix C.
8.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage)
Rate), shall comply with the requirements of Appendix D.
9 Quantitation limit and recovery rate
9.1 Limit of limits
The limiting limit of the method for atrazine is 0.02 mg/kg, the volatilization limit for vinifera is 0.02 mg/kg,
Is 0.02 mg/kg, the fluconazole quantification limit is 0.38 mg/kg, the limit of the inhibin is 0.05 mg/kg, and the limit of the restriction is
0.01 mg/kg, the limit of halothiazole was 0.05 mg/kg, the limit of chlorphenolic alcohol was 0.02 mg/kg,
Is 0.5 mg/kg.
9.2 Recovery
The addition rates of the nine heterocyclic pesticides in tea are shown in Appendix B when different levels are added.
Appendix A
(Informative)
Standard chromatogram
18.41 min - atrazine
21.09 min-vinyl mushroom
25.46 min - Pythium
25.67 min-fluconazole
27.33 min-imazalazole
28.30 min-buprofezin
32.20 min, 32.58 min-propiconazole
39.12 min-chlorophenyl pyruvate
41.64 min-da acarb
Figure A.1 SIM chromatograms of nine heterocyclic pesticide standards
Appendix B
(Informative)
Addition Recovery Rate of 9 Kinds of Heterocyclic Pesticides in Tea
Table B.1 Recovery rates of nine heterocyclic pesticides in tea
Pesticide name Add concentration/(mg/kg) Recovery rate /% Pesticide name
Add concentration /
(Mg/kg)
Recovery rate/ %
Atrazine
0.02 89.5-99.2
Vinyl fungus
0.02 80.1-89.7
0.2 90.4-96.4 0.2 79.5-86.7
2.0 92.3-111.4 2.0 94.8-105.4
Pythium
0.02 93.5-97.3
Fluorobenzazole
0.38 80.2-87.9
0.2 92.3-96.6 3.0 78.9-84.4
2.0 92.5-98.5 30 76.6-87.9
Antimycin
0.05 78.8-85.6
Buprofezin
0.01 95.1-99.3
0.5 75.1-83.8 0.1 93.5-99.8
5.0 72.6-79.6 1.0 94.4-103.5
Propiconazole
0.05 81.1-91.7
Chlorophenylpyrimidinol
0.02 96.9-112.4
0.5 95.7-108.2 0.2 103.5-116.2
5.0 96.4-105.8 2.0 99.2-106.7
Pyridaben
0.25 88.6-94.1
2.5 90.2-94.8
20 87.2-93.8
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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