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GB 23200.103-2016 English PDF

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GB 23200.103-2016: Food safety national standard -- Determination of Residual Amidamidine and Its Metabolites in Royal Jelly by Gas Chromatography -- Mass Spectrometry
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GB 23200.103-2016English199 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of Residual Amidamidine and Its Metabolites in Royal Jelly by Gas Chromatography -- Mass Spectrometry Valid GB 23200.103-2016

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Basic data

Standard ID GB 23200.103-2016 (GB23200.103-2016)
Description (Translated English) Food safety national standard -- Determination of Residual Amidamidine and Its Metabolites in Royal Jelly by Gas Chromatography -- Mass Spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 10,117
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2574-2010
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 23200.103-2016: Food safety national standard -- Determination of Residual Amidamidine and Its Metabolites in Royal Jelly by Gas Chromatography -- Mass Spectrometry


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Food safety national standard - Determination of Residual Amidamidine and Its Metabolites in Royal Jelly by Gas Chromatography - Mass Spectrometry National Standards of People's Republic of China GB Replace SN/T 2574-2010 National standards for food safety Determination of Residual Amidamidine and Its Metabolites in Royal Jelly Gas chromatography - mass spectrometry National food safety standards- Determination of amitraz 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 2574-2010 "Import and export royal jelly in the double amidine and its metabolites Residue detection method Gas chromatography - Mass spectrometry ". Compared with SN/T 2574-2010, 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 2574-2010. National standards for food safety Determination of Residual Amidamidine and Its Metabolites in Royal Jelly by Gas Chromatography - Mass Spectrometry

1 Scope

This standard specifies the determination and confirmation of the method for the determination of amitraz and its metabolites in royal jelly by gas chromatography-mass spectrometry. This standard applies to royal jelly in the double amidine and its metabolites residue determination and confirmation, 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 samples were acid-hydrolyzed and alkalized with n-hexane-diethyl ether (2 1, volume ratio) mixed solvent extraction, acid, lye-liquid distribution purification, gas phase Chromatography - mass spectrometry and confirmation, 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 n-hexane (C6H14). chromatographic purity. 4.1.2 ether (C4H10O). pure chromatography. 4.1.3 Acetone (C3H6O). Chromatographic pure. 4.1.4 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 hydrochloric acid solution (2.0 mol/L). with a pipette to remove 90 mL of hydrochloric acid, diluted with water to 500mL. 4.2.2 sodium hydroxide solution (10 mol/L). Weigh 40 g of sodium hydroxide, dissolved in water to 100mL. 4.3 standards 4.3.1 Amitraz (amitraz, C19H23N3, CAS No. 33089-61-1, molecular weight 293) Standard substance. purity > 99%. 4.3.2 2,4-Dimethyl aniline (C8H11N, CAS No. 95-68-1, molecular weight. 121) Reference substance. Purity > 99%. 4.4 standard solution preparation 4.4.1 Amitrazine standard solution. accurately weighed the appropriate amount of formamidine standard material, with acetone dubbed the concentration of 100 g/mL standard stock solution. According to the need to use acetone diluted to the appropriate concentration of standard working fluid. Store in 4 ℃ refrigerator. 4.4.2 2,4-dimethylaniline standard solution. accurately weighed the appropriate amount of 2,4-dimethyl aniline standard material, with acetone dubbed the concentration of 100 g/mL standard stock solution. According to the need to use acetone diluted to the appropriate concentration of 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 5 000 r/min. 5.5 sets of thermostat. 50 ℃ ~.200 ℃. 5.6 full glass reflow device.

6 Preparation and storage of samples

Approximately 500 g of the representative sample was added, stirred vigorously, placed in a clean container, sealed, and marked with the sample at -18C Frozen. During sample and sample preparation, contamination of the sample or changes in the residue content should be prevented. Note. The above sample sampling site according to GB 2763 Appendix A implementation.

7 Analysis steps

7.1 hydrolysis Weigh 4 g of sample (accurate to 0.01 g) in a 100 mL flask and add 15 mL of hydrochloric acid solution (4.5) to mix on a vortex mixer. Install the reflux condenser, heat reflux at 120 ℃ for 2 h, stop heating, continue to cool water at room temperature for 15min, move to the ice bath to cool 15min. 7.2 Extraction and purification Transfer the hydrolyzate to a 50 mL stoppered centrifuge tube with 10 mL of n-hexane-diethyl ether (2 1, by volume) mixed solvent plus 4 ML of sodium hydroxide solution, vortex and mix well, cooled in ice bath for 5 min, centrifuged at 4000 r/min for 3 min. Transfer the upper organic phase to another A 50 mL stopper with a centrifuge tube. The aqueous phase was extracted twice with a mixed solvent of 2 x 10 mL n-hexane-diethyl ether (2 1, v/v). Merge the upper layer The organic phase. With 2 × 5 mL hydrochloric acid solution extraction 2 times, combined with hydrochloric acid extract and constant volume to 10mL, take 5mL hydrochloric acid extract in 10 mL With a plug in the centrifuge tube. Add 2 mL of n-hexane - acetone (2 1, volume ratio) mixed solvent, 2 mL of sodium hydroxide solution extraction 1, centrifugal Layer, upper organic phase for gas chromatography - mass spectrometry, 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) Carrier gas. helium, purity greater than or equal 99.999%, flow rate. 1.0 mL/min; D) Injection volume. 2 μL; E) Injection method. pulse splitless injection, pulse pressure 25 psi ,, 0.75 min after the opening valve; F) solvent delay time. 8 min; G) Inlet temperature. 250 ° C; H) Interface temperature. 280 ° C; L) solvent delay time. 8 min; J) ion source. electron bombardment source (EI); K) ionization energy. 70 eV; L) Determination of the way. select the ion monitoring mode; M) Select the ion and relative abundance. see Table 1. Table 1 Selective ion and relative abundance of 2,4-dimethylaniline Select ion (m/z) 121 (quantitative) 120 77 Relative abundance (%) 100 85.2 21.3 7.3.2 Quantitative determination According to the sample solution 2,4-dimethyl aniline content of the situation, selected with the sample of 2,4-dimethyl aniline concentration similar to the standard working solution liquid. The reaction value of the 2,4-dimethylaniline in the standard working solution and the sample solution should be within the linear range of the instrument. Standard working solution and sample solution Equal volume interspersed injection assay. Under the above chromatographic conditions, the retention time of 2,4-dimethylaniline is about 10.0 mim, and the total Subflow diagram See 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) There was 2,4-dimethylaniline in the sample. The confirmed sample can be judged as 2,4-dimethylaniline positive detection. 2,4-dimethylaniline The spectrum of the standard is shown in Figure A.2 in Appendix A. 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

The residual content of formamidine in the sample was calculated by chromatographic data processing software or by formula (1) 1.21 × A × c × V X = (1) AS x m Where. 1.21 - conversion factor for the molecular weight of bisformamidine from the molecular weight of 2,4-dimethylaniline. X - Residue of formamidine in milligrams per kilogram (mg/kg); A - the peak area of 2,4 - dimethylaniline in the sample solution; C - the concentration of 2,4-dimethylaniline in standard working solution, in micrograms per milliliter (g/mL); V - Final volume of volume in milliliters (mL); AS - standard working area of 2,4 - dimethylaniline peak area; 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 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 Appendix D 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 recovery of this method is given in Appendix B.

Appendix A

(Informative) Chromatograms and spectra Figure A.1 Total ion chromatogram of the 2,4-dimethylaniline standard (concentration 0.01 j/mL) Figure A.2 Mass spectrum of 2,4-dimethylaniline standard substance

Appendix B

(Informative) Sample concentration and recovery of the experimental data Table B.1 Experimental data on the concentration and recovery of the sample Compound added concentration/(mg/kg) Recovery /% Precision /% Formamidine 0.01 76.7% to 88.2 9.8 0.02 76.9 to 88.0 10.2 0.05 78.4 to 90.4 9.0

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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