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Food safety national standard -- Determination of residues of acaricides in royal jelly by gas chromatography -- Mass spectrometry
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GB 23200.101-2016
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Basic data | Standard ID | GB 23200.101-2016 (GB23200.101-2016) | | Description (Translated English) | Food safety national standard -- Determination of residues of acaricides in royal jelly by gas chromatography -- Mass spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 12,152 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 2571-2010 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.101-2016: Food safety national standard -- Determination of residues of acaricides in royal jelly by gas chromatography -- Mass spectrometry ---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 - Determination of residues of acaricides in royal jelly by gas chromatography - mass spectrometry
National Standards of People's Republic of China
GB
Replace SN/T 2571-2010
National standards for food safety
Determination of Residues of Acaricides in Royal Jelly
Gas chromatography - mass spectrometry
National food safety standards-
Determination of multiple miticide residues in royal-jelly
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 Administration of Food and Drug Administration
Foreword
This standard replaces SN/T 2571-2010 "Import and export royal jelly in a variety of acaricide residues detection method of gas chromatography - mass spectrometry."
Compared with SN/T 2571-2010, the main changes are as follows.
- Standard text format is modified to national standard text format for food safety;
- standard name "import and export royal jelly" to "royal jelly";
- increase the "other food reference implementation" in the standard range.
This standard replaced the previous version of the standard release.
-SN/T 2571-2010.
National standards for food safety
Determination of residues of acaricides in royal jelly by gas chromatography - mass spectrometry
1 Scope
This standard provides the royal jelly in the mite ether, methyl grams of mites, acaricides, lei mites, ethyl keto mite, brom mite, dicofol,
Determination and Confirmation of Residue of Pyridenopsis by Gas Chromatography - Mass Spectrometry.
This standard applies to royal jelly in the acaricidal ether, methyl grams of mites, acaricides, lei acarics, ethyl methicillin, bromide mites, dicofol,
Determination and confirmation of residues of pyridaben 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 residue of the acaricide in the sample was extracted with a mixed solvent of n-hexane acetone (1 1, v/v), purged with a Florisil column, and the gas phase
Spectral - mass spectrometry - negative chemical source determination, 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 ether (C4H10O). pure chromatography.
4.1.2 n-hexane (C6H14). pure chromatography.
4.1.3 Acetone (C3H6O). Chromatographic pure.
4.1.4 Sodium chloride (NaCl).
4.1.5 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve.
4.2 standards
4.2.1 acaricidal mite, methyl acaricides, acaricides, deer mites, ethyl methicillin, bromocarbide, dicofol,
Purity ≥99%, see Appendix A.
4.3 standard solution preparation
4.3.1 acaricides, methyl methicillin, acaricides, lemi mite, ethyl methicillin, bromide mite, dicofol,
Solution. Weigh the appropriate amount of standard material accurately, with n-hexane dubbed the concentration of 100 μl/mL standard stock solution. Store in 4 ℃ refrigerator.
4.3.2 acaricides, methicillin mites, acaricides, lei mites, ethyl methicillin, bromocarbide, dicofolidone, pyridaben standard work
Liquid. Dilute the mixture with n-hexane to the appropriate concentration of the standard working solution. Store in 4 ℃ refrigerator.
4.4 Materials
4.4.1 Florisil Solid Phase Extraction Column. (1 g, 6 mL) or equivalent. Use a 10 mm high anhydrous sodium sulphate layer in the front column with 5 mL
N - hexane elution activated solid phase extraction.
5 instruments and equipment
5.1 Gas Chromatography-Mass Spectrometer. Negative Chemical Source (NCI).
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 vortex mixer.
5.4 Centrifuge. speed greater than 5 000 r/min.
5.5 nitrogen blowing instrument.
5.6 Rotary evaporator.
6 Preparation and storage of samples
Take about 500g of the sample, the sampling site according to GB 2763 Appendix A implementation, will be forced to stir evenly, into a clean container,
Sealed and marked with the mark, and the sample was stored at -18 ° C.
During sample and sample preparation, contamination of the sample or changes in the residue content should be prevented.
7 Analysis steps
7.1 Extraction
Weigh 2 g sample (accurate to 0.01 g) in 50 mL centrifuge tube, add 10 mL water vortex mixed 1 min, standing 5 min. Join
20 mL of n-hexane acetone (1 1, volume ratio) mixed solvent, vortex mixed for 1 min, centrifuged at 4000 r/min for 3 min, the upper organic
Phase transferred into the concentration bottle. Add 10 mL of n-hexane acetone (1 1, volume ratio) mixed solvent, repeat the extraction time, combined
The upper organic phase, in 45 ℃ below the water bath under reduced pressure to near dry, to be purified.
7.2 Purification
The residue in the concentrated flask was washed twice with 3 mL of n-hexane and transferred to a Florisil solid phase extraction column. With 5 mL of n-hexane
The effluent was discarded and eluted with 10 mL of n-hexane + ether (8 + 2, v/v) mixed solvent. The eluate was collected in 10 mL of glass off
Tube in the 45 ℃ water bath with nitrogen blowing instrument slowly blowing to near dry, with n-hexane dissolved and set to 0.5mL, gas chromatography-mass spectrometry.
7.3 Determination
7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions
A) Column. DB-5ms quartz capillary column, 30 m x 0.25 mm (id) x 0.25 μm, or equivalent;
B) column temperature. 50 ℃ for 1 min, at 20 ℃/min heating rate rose to 220 ℃, keep 1 min,
The temperature was raised to 250 ° C at a rate of 5 ° C/min and raised to 280 ° C at a rate of 20 ° C/min for 8 min.
C) Inlet temperature. 250 ° C;
D) chromatographic - mass spectrometer interface temperature. 280 ° C;
E) Carrier gas. helium, purity greater than or equal to 99.999%; flow rate 1.0 mL/min;
F) Injection volume. 2 μL;
G) Injection method. splitless injection, 1.5 min after the opening valve;
H) ionization mode. NCI;
I) ionization energy. 184 eV;
J) ion source temperature. 150 ° C;
K) quadrupole temperature. 150 ° C;
L) Reaction gas. methane, purity greater than or equal to 99.99%, reaction gas flow rate. 2 mL/min;
M) Measurement method. Select the ion monitoring mode (SIM);
N) solvent delay time. 10 min;
O) Select the ion measurement. each compound selected a quantitative ion, 2-3 qualitative ions. Each group needs to be measured
Sub-according to the peak order, respectively, time points were measured. The retention time of each compound, the quantitative ion, the qualitative ion and the quantitative ion and qualitative
The abundance of ions is given in Appendix B.
7.3.2 Quantitative determination
According to the content of acaricide in the sample solution, the standard working solution with similar peak area is selected. Standard working solution and sample solution of acaricides
The value should be within the linear range of the instrument determination. Standard working solution and sample volume and other volume interspersed injection determination. Under the above chromatographic conditions, 8 species
The retention time of the acaricides is given in Appendix B, and the total ion current of the standard is shown in Appendix C, C.1.
7.3.3 Qualitative determination
The standard solution and sample solution are determined according to the conditions specified in 7.3.1, if the sample solution and the standard solution in the same retention time peak
Now, it is confirmed by mass spectrometry, after deducting the background of the sample spectrum, the selected ions all appear, while the selected ion from the
The abundance ratio is consistent with the relative abundance of the ions associated with the standard, and the fluctuation range is within the maximum allowable deviation of Table 1 (see Table 1)
The substance is present in the sample.
Table 1 Mass Spectrum Relative Ion Abundance Maximum Allowable Deviation
Relative ion 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 determination steps.
8 results are calculated and expressed
Use the chromatographic data processing software or calculate the residual content of various acaricides in the sample according to formula (1).
A × c × V
X = ---------------------- (1)
AS x m
Where.
X. Residue of various acaricides in the sample in milligrams per kilogram (mg/kg);
A) the area of various acaricidal agents in the sample solution;
C - the concentration of various acaricides in standard working fluid, in micrograms/ml (g/mL);
V - Final volume of the final volume in milliliters (mL);
AS - standard acupoints in standard working fluids;
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 determinations obtained under reproducibility and its arithmetic mean (percentage) shall be in accordance with
Appendix F requirements.
10% limit and recovery rate
10.1 Quantitation limits
The quantification limit of this method is. 0.01 mg/kg.
10.2 Recovery rate
The experimental data on the concentration and recovery of the sample are given in Appendix D.
Appendix A
(Informative)
8 kinds of acaricides pesticides in English generic name, chemical formula, CAS number information
Table A.1 8 kinds of acaricides pesticides in English common name, chemical formula, CAS No. information
Chinese generic name English generic name chemical molecular formula CAS number
Acetylidene Chlorbenside C13H10 Cl2 S 269 103-17-3
Mycobacterium acaricides Quinomethionate C10H6N2OS2 234 2439-01-2
Acetylate Chlorfenson C12H8Cl2O3 S 302 80-33-1
Phytophthora
Ethyl Acetone Chlorobenzilate C16H14Cl2O3 324 510-15-6
Bromopropylate C17H16Br2O3 426 18181-80-1
Dicofolone Tetradifon C12H6 Cl4 O2S 354 116-29-0
Pyridaben C19H25ClN2OS 364 96489-71-3
Appendix B
(Informative appendix)
Retention time of 8 kinds of acaricides, quantitative ions, qualitative ions and relative abundance
Table B.1 Retention times, quantitative ions, qualitative ions and relative abundance of eight acaricides
Pesticide name quantitative ion qualitative ion 1 qualitative ion 2 qualitative ion 3
keep time
(Min)
Acaricides 143 (100) 144 (7.7) 145 (36.1) 13.5
Mycobacterium mites 206 (100) 207 (12.8 208 (11.8) 13.6
Acaricides
175 (100) 176 (8.3) 177 (38.9) 14.0
Lychee mite 223 (100) 224 (16.1) 239 (46.6) 14.6
Ethyl Ester
324 (100) 326 (68.2) 278 (34.5) 262 (40.2) 15.1
Bromide mites
428 (100) 426 (51.) 430 (50.4) 17.5
Diclofenac
320 (100) 318 (75.4) 356 (43.9) 18.1
Pyridaben
217 (100) 219 (39.1) 218 (15.8) 19.8
Appendix C
(Informative)
Total ion flow chart of 8 kinds of acaricides standard materials
Figure C.1 Total ion chromatogram of eight species of acaricides
1. Acaricidal ether 2. Methylk acaricides 3. Fungicides 4. Lecture dex mite 5 Ethyl ester Mites 4. Bromothylate
7. Diclofenac 8
Appendix D
(Informative)
Sample concentration and recovery of the experimental data
Table D.1 Experimental data on the concentration and recovery of the sample
Pesticide name added concentration
(Mg/kg)
Recovery rate
Precision degree
Pesticide name Add concentration (mg/kg) Recovery rate
Precision degree
Acaricides 0.01 86.7 ~ 112 11.2 ethyl ester acaricides
0.01 77.5 to 113 6.8
0.02 94 to 112 8.6 0.02 84.0 to 104 7.9
0.05 81.2 to 107 9.3 0.05 72.6 to 107 4.5
Methyl killer
0.01 82.1 ~ 118 9.6 Bromo mite 0.01 71.3 ~ 115 13.0
0.02 76.8 to 107 10.2 0.02 78.0 to 114 11.8
0.05 79.4 to 102 7.5 0.05 73.6 to 106 10.8
Acaricidal ester 0.01 79.7 ~ 118 13.1 dicofol
0.01 76.7 to 115 6.9
0.02 85.0 to 110 12.6 0.02 75.0 to 107 7.6
0.05 74.4 to 109 10.8 0.05 74.8 to 108 8.9
Lymanthamidae 0.01 69.1 to 108 14.1 Pyridinidone 0.01 78.2 to 118 8.4
0.02 76.5 to 108 10.6 0.02 75.0 to 109 9.8
0.05 77.4 to 109 13.1 0.05 78.8 to 109 12.3
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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