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GB 23200.102-2016: Food safety national standard -- Determination of the content of chlordimeform and its metabolites in royal jelly by gas chromatography-mass spectrometry
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Food safety national standard -- Determination of the content of chlordimeform and its metabolites in royal jelly by gas chromatography-mass spectrometry
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GB 23200.102-2016
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Basic data | Standard ID | GB 23200.102-2016 (GB23200.102-2016) | | Description (Translated English) | Food safety national standard -- Determination of the content of chlordimeform and its metabolites in royal jelly by gas chromatography-mass spectrometry | | Sector / Industry | National Standard | | Classification of Chinese Standard | G25 | | Word Count Estimation | 11,147 | | Date of Issue | 2016-12-18 | | Date of Implementation | 2017-06-18 | | Older Standard (superseded by this standard) | SN/T 2573-2010 | | Regulation (derived from) | State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16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 23200.102-2016: Food safety national standard -- Determination of the content of chlordimeform and its metabolites in royal jelly by gas chromatography-mass spectrometry
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Food safety national standard - Determination of the content of chlordimeform and its metabolites in royal jelly by gas chromatography
National Standards of People's Republic of China
GB
Replace SN/T 2573-2010
National standards for food safety
Determination of the Residue of Ampicamidine and Its Metabolites in Royal Jelly
Gas chromatography - mass spectrometry
National food safety standards-
Determination of chlordimeform and its metabolites 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 2573-2010 "Import and export royal jelly in the detection of chlordimeform and its metabolites Residue Determination of gas chromatography -
Mass spectrometry ".
Compared with SN/T 2573-2010, 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 2573-2010.
National standards for food safety
Determination of the content of chlordimeform and its metabolites in royal jelly by gas chromatography - mass spectrometry
1 Scope
This standard specifies the determination and confirmation of the content of chlordimeform and its metabolites in royal jelly by gas chromatography-mass spectrometry.
This standard applies to the determination and confirmation of the residual amount of chlordimeform and its metabolites in royal jelly, and other foodstuffs can be used for reference.
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 samples were precipitated with trichloroacetic acid solution and extracted under basic conditions with n-hexane-acetone (1 1, v/v) mixed solvent.
The liquid was purified by gas chromatography - mass spectrometry and confirmed by external hexane - acetonitrile.
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 (C2H3N). Chromatographic pure.
4.1.2 Acetone (C3H6O). Chromatographic pure.
4.1.3 n-hexane (C6H14). chromatographic purity.
4.1.4 Trichloroacetic acid (CCl3COOH).
4.1.5 Sodium hydroxide (NaOH).
4.1.6 sodium chloride (NaCl). 650 ℃ burning 4 h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve.
4.2 solution preparation
4.2.1 n-Hexane - Acetone (1 1, volume ratio) mixed solvent. take 100 mL of n-hexane, add 100 mL of acetone, shake back.
4.2.2 Trichloroacetic acid solution (5%). Weigh 5 g of trichloroacetic acid, add water and set to 100 ml.
4.2.3 Sodium hydroxide solution (2 mol/L). Weigh 8 g of sodium hydroxide into 100 ml of distilled water.
4.3 standards
4.3.1 Chlordimeform, C10H13ClN2, CAS No. 6164-98-3, molecular weight 196.68) Reference substance. pure
Degree > 98.5%.
4.3.2 4-Chloro-2-methylaniline, C7H8ClN, CAS No. 95-69-2, molecular weight. 141.60)
Standard substance. purity > 98.5%.
4.4 standard solution preparation
4.4.1 Accurately weigh the appropriate amount of chlordimeform and 4-chloro-o-methylaniline standard substance, with a single standard storage solution with a concentration of 100 g/mL
Preparation of liquid. According to the need to use acetone diluted mixed to the appropriate concentration of mixed standard working fluid. Store in 4 ℃ refrigerator.
5 instruments and equipment
5.1 Gas Chromatography-Mass Spectrometer. Equipped with an electron impact source (EI).
5.2 Analysis of balance. 0.01 g and 0.0001 g.
5.3 vortex mixer.
5.4 Centrifuge. speed greater than 10000 r/min.
5.5 Rotary evaporator.
6 Preparation and storage of samples
Take about 500 g of the sample, the sample sampling site according to GB 2763 Appendix A implementation, will be forced to stir evenly, into the clean container
Inside, sealed, and marked with the mark, the sample stored at -18C frozen.
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 of sample (accurate to 0.01 g) in 50 mL centrifuge tube, add 10 mL of trichloroacetic acid solution vortex mixed for 1 min to 8 000 r/min
Centrifuge 3 min. The upper aqueous phase was transferred to another 50 mL centrifuge tube, plus about 4 mL of sodium hydroxide solution adjusted to pH greater than 12. Add 5 g
Sodium chloride and 20 mL of n-hexane-acetone (1 1, volume ratio) were mixed and vortexed for 1 min to transfer the upper organic phase into a concentrated flask.
The addition of 20 mL of n-hexane-acetone (1 1, volume ratio) in the aqueous phase was repeated and the extraction was repeated once. The upper organic phase was combined at 45 ° C
The bath is concentrated under reduced pressure to near dryness, to be purified.
7.2 Purification
The residue in the concentrated flask was washed twice with 10 mL of acetonitrile and transferred to a 50 mL centrifuge tube. 10 ml of n-hexane was added and the vortex was mixed
Min, centrifuged at 3 000 r/min for 3 min, the upper n-hexane phase was transferred to another 50 mL centrifuge tube, 10 mL of n-hexane was added to the acetonitrile phase,
The operation was repeated once and the n-hexane phase was combined. Add 10 mL of acetonitrile, vortex mixing 1 min, 3000 r/min centrifugal 3 min, discard the upper layer is
Hexane phase. Combined acetonitrile phase, in 45 ℃ below the water bath under reduced pressure to near dry, dissolved with acetone and set to 1.0 mL, with gas chromatography - quality
Spectral determination, external standard method.
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 2 min, at 10 ℃/min heating rate rose to 160 ℃, keep 1 min to 30 ℃/min
Of the heating rate rose to 320 ℃, keep 5min;
C) Inlet temperature. 250 ° C;
D) Carrier gas. helium, purity greater than or equal 99.999%, flow rate, 1.0 mL/min;
E) Injection volume. 2 μL;
F) Injection mode. pulse splitless injection, pulse pressure 25 psi, 0.75 min after the opening valve;
G) solvent delay time. 10 min;
H) ion source. electron bombardment source (EI);
I) Interface temperature. 280 ° C;
J) Ionization energy. 70 eV;
K) ion source temperature. 280 ° C;
L) Determination of the way. select the ion monitoring mode;
M) Select the ion and relative abundance. see Table 1.
Table 1 Quantitative ion, qualitative ion and relative abundance of chlordimeform and 4-chloro-o-toluidine
Pesticide name Quantitative ion - Qualitative ion 1 Qualitative ion 2
Chlordimeform 196 (100) 181 (85.4) 152 (54.1)
4-Chloro-o-toluidine 141 (100) 77 (25.8) 143 (34.1)
7.3.2 Quantitative determination
According to the sample solution of chlordimeform and 4-chloro o-toluidine content of the case, selected with the sample solution of chlordimeform and 4-chloro o-toluidine concentration similar to the standard
Quasi-working solution. The response values of the pesticide and 4-chloro-o-toluidine in the standard working solution and the sample solution should be within the linear range determined by the instrument. Standard work
As a solution and sample volume of the same interspersed injection determination. Under the above chromatographic conditions, the retention times of chlordimeform and 4-chloro-o-toluidine were approximately
15.0 min, 12.0 min, the total ion chromatogram of the standard is shown in Appendix A, Figure A.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 2 (see Table 2)
The presence of chlordimeform and 4-chloro-o-toluidine in the sample. The confirmed samples can be identified as chlordimeform and 4-chloro-o-toluidine positive detection. Chlordimeform and
The mass spectrum of the 4-chloro-o-toluidine standard is shown in Appendix A, Figure A.2, Figure A.3.
Table 2 Mass Spectrometry Relative Ion Abundance Maximum Allowable Deviation
Relative ion abundance (% base) > 50% > 20% to 50% > 10% to 20% ≤10%
Allowable relative error ± 10% ± 15% ± 20% ± 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 chlordimeform or 4-chloro-o-toluidine in the sample according to formula (1)
A × C × V
X = (1)
AS x m
Where.
X - Residue of chlordimeform or 4 - chloro - o - toluidine in milligrams per kilogram (mg/kg);
A - the peak area of chlordimeform or 4-chloro-o-toluidine in the sample solution;
C - the concentration of chlordimeform or 4-chloro-o-toluidine in standard working solution in micrograms per milliliter (g/mL);
V - Final volume of volume in milliliters (mL);
AS - standard working solution area of chlordimeform or 4 - chloro - o - toluidine;
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 C 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 the
Record the requirements of D.
10% limit and recovery rate
10.1 Quantitation limits
The quantitative line of this method for chlordimeform and 4-chloro-o-toluidine is 0.01 mg/kg.
10.2 Recovery rate
The experimental data on the concentration and recovery of the sample are given in Appendix B.
Appendix A
(Informative)
Chromatograms and spectra
Figure A.1 Total ion chromatogram of chlordimeform and 4-chloro-o-toluidine
1. 4-Chloro-o-toluidine 2. Chlordimeform (concentration 0.02 μg/mL)
Figure A.2 EI spectrum of chlordimeform
Figure A.3 EI spectra of 4-chloro-o-toluidine
Appendix B
(Informative)
Sample concentration and recovery of the experimental data
Table B.1 Experimental data on the concentration and recovery of the sample
Pesticide name Add concentration (mg/kg) Recovery rate range% Precision range%
Chlordimeform
0.01 86.7 to 112 10.8
0.02 91.0 to 112 9.5
0.05 81.2 ~ 107 11.6
4-Chloro-o-toluidine
0.01 82.1 to 118 8.9
0.02 85.5 to 107 9.1
0..05 79.4 ~ 102 12.3
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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