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GB 23200.23-2016 English PDF

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GB 23200.23-2016: Food safety national standard -- Determination of duliphenol residues in food by liquid chromatography-mass spectrometry / mass spectrometry
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GB 23200.23-2016English219 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of duliphenol residues in food by liquid chromatography-mass spectrometry / mass spectrometry Valid GB 23200.23-2016

PDF similar to GB 23200.23-2016


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Basic data

Standard ID GB 23200.23-2016 (GB23200.23-2016)
Description (Translated English) Food safety national standard -- Determination of duliphenol residues in food by liquid chromatography-mass spectrometry / mass spectrometry
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 11,157
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2457-2010
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 23200.23-2016: Food safety national standard -- Determination of duliphenol residues in food by liquid chromatography-mass spectrometry / mass spectrometry


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Food safety national standard - Determination of duliphenol residues in food by liquid chromatography - mass spectrometry/mass spectrometry National Standards of People's Republic of China GB Instead of SN/T 2457-2010 National standards for food safety Determination of duliphenol residues in food Liquid chromatography - mass spectrometry/mass spectrometry National food safety standards- Determination of dinoseb 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 GB 23200.24-2016

Foreword

This standard replaces SN/T 2457-2010 "Determination of duliphenol residues in import and export food by liquid chromatography-mass spectrometry". Compared with SN/T 2457-2010, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name 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 2457-2010. GB 23200.24-2016 National standards for food safety Determination of duliphenol residues in food by liquid chromatography - mass spectrometry/mass spectrometry

1 Scope

This standard specifies the method of liquid chromatography-mass spectrometry/mass spectrometry for the determination of dolphol residues in food. This standard applies to apple, chestnut, cabbage, beef, honey, wheat, chicken, ginger, tea, soy and milk in the residual The amount of detection 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 residual levophenols in the samples were extracted with acetonitrile and purified by gel permeation chromatography. The samples were identified by liquid chromatography-mass spectrometry/mass spectrometry. the amount.

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 (CH3CN), high performance liquid chromatography grade. 4.1.2 Methanol (CH3OH), high performance liquid chromatography grade. 4.1.3 Cyclohexane (C6H12). 4.1.4 Ethyl acetate (C4H8O2). 4.1.5 Sodium chloride (NaCl). 4.2 solution preparation 4.2.1 Ethyl acetate-cyclohexane (1 1, volume ratio). Equal volume of ethyl acetate and cyclohexane are miscible. 4.3 standards 4.3.1 Diphenols standard. Molecular formula, C10H12N2O5; CAS 88-85-7; purity ≥ 99%. 4.4 standard solution preparation 4.4.1 duliphenolic standard stock solution. accurately weighed the amount of Diphenols standard, with methanol prepared into 100 μg/mL standard stock solution, -18 ℃ below the storage. The 4.4.2 Dulu phenolic standard working solution. accurately absorb the appropriate amount of levophenol standard stock solution, diluted with methanol to the required concentration, -18 ℃ The following storage. 4.5 Materials 4.5.1 0.22 μm organic filter.

5 instruments and equipment

5.1 Liquid Chromatography-Mass Spectrometry/Mass Spectrometer. Equipped with electrospray ion source. 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Centrifuge tube. glass, 50 mL. 5.4 Gel Permeation Chromatography. 5.5 Scroll Mixer. 5.6 Homogenizer. 5.7 Centrifuge. 5.8 Rotary evaporator. 5.9 nitrogen dryers. GB 23200.24-2016

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 fruits, vegetables, nuts Fruit, nuts. take the sample about 500 g, crushed with a pulverizer, into a clean container as a sample, sealed and do a good job. 6.1.2 grain, tea Take about 500 g of the sample and crush it all through a 20 mesh sieve into a clean container as a sample, seal and mark it. Warm preservation. 6.1.3 Meat products Take a representative sample of about 500 g, crushed with a pulverizer, into a clean container as a sample, sealed and labeled. 6.1.4 honey Take a representative sample of about 500 g, the amorphous sample will be forced to stir evenly, there are crystallization of the sample can be sealed after the sample cap, Placed in a water bath of not more than 60 ℃, until the sample all dissolved and stir well, quickly cooled to room temperature. The prepared sample is packed in a clean container Sealed and identified. 6.1.5 milk Take a representative milk or milk powder sample, mix well and mark it. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Save Fruits, vegetables, nuts, meat products, milk and other samples in -18 ℃ below the frozen preservation; grain, tea, honey and other samples in the room Keep the temperature away from light. During the sample preparation operation, it is necessary to prevent the sample from being contaminated or the change in the content of the residue.

7 measurement steps

7.1 Extraction Approximately 2.5 g of the sample of the tea leaves and about 5 g (accurate to 0.01 g) of the other substrate samples in a 50 mL centrifuge tube (3 mL Water, so that the sample is fully wetted), adding 25 mL of acetonitrile and 5 g of sodium chloride to 10 000 r/min homogenization 2 min, centrifuged at 4000 r/min for 10 min, The supernatant was transferred to a 25 mL colorimetric tube and fixed to 25 mL with acetonitrile. 7.2 Purification 7.2.1 Gel Permeation Chromatographic Conditions A) Purification column S-X3 Bio-Beads filler, particle size 38 μm -75 μm,.200 mm × 22 mm (inner diameter), or equivalent; B) mobile phase. ethyl acetate-cyclohexane, flow rate. 5 mL/min; C) Injection volume. 5 mL; D) Purification procedure. 0 min-10.5 min The eluent was discarded and the eluate was collected at 10.5 min-15 min. 7.2.2 Purification process Accurately remove 5 mL of the above set of liquid, water bath at 45 ℃ nitrogen flow to near dry, constant volume to 10 mL, take 5 mL of ethyl acetate - The alkane solution was purified by gel permeation chromatography under the conditions of 6.2.1. The collected eluate was concentrated on a 45 ° C water bath to dryness and accurately added Into 1 mL of methanol dissolved residue, dissolved solution over 0.22 μm organic filter for liquid chromatography-mass spectrometry/mass spectrometry. 7.3 Determination 7.3.1 Liquid Chromatographic Reference Conditions A) Column. C18 150 mm × 2.1 mm (inner diameter), particle size 5 μm, or equivalent; B) Column temperature. 30 ° C; C) Injection volume. 5 μL. D) mobile phase gradient and flow rate in Table 1. Table 1 Liquid Chromatography Gradient Elution Conditions Time (min) 0.1% acetic acid is water soluble liquid(%) Acetonitrile (%) Flow rate (μL/min) 0.0 30 70.200 4.0 30 70.200 5.0 10 90.200 6.0 10 90.200 GB 23200.24-2016 6.1 30 70.200 8.0 30 70.200 7.3.2 Mass spectrometry reference conditions A) ion source. electrospray ion source (ESI); B) scanning mode. negative ion scanning mode; C) See Appendix A for other reference mass spectrometry conditions. 7.3.3 Quantitative determination According to the content of the sample in the sample solution, select the standard response value similar to the working fluid. Standard working solution and the analyte in the sample solution The values shall be within the linear range of the instrument. The standard working solution and sample solution volume measurement. Under the above chromatographic conditions The reference retention time of levophenol is about 4.55 min. The standard multi-reaction monitoring chromatogram of dinomyol is shown in Appendix B. 7.3.4 Qualitative determination When the sample is measured, if the mass retention time of the detected mass is consistent with that of the standard sample, and the sample spectrum after subtracting the background , The relative abundance of the qualitative ions is close to the concentration of the matrix under the same conditions obtained under the standard solution spectrum, the error does not exceed the table Set the range, you can determine the existence of the corresponding sample in the sample. Table 2 The maximum allowable error of relative ion abundance when qualitative confirmation Relative abundance (base) 50% 20% to 50% 10% to 20% ≤10% Allowable relative deviation ± 20% ± 25% ± 30% ± 50% 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 the following formula (1) to calculate the content of dariphenol in the sample. X = MA VcA S   ..(1) Where. X - the content of duliphene in the sample, in micrograms per kilogram, μg/kg; A - the peak area of dolphins in the sample solution; C - the concentration of dinol in the standard solution, in ng/ml for ng/ml; V - the final volume of the sample solution, in milliliters, mL; As - standard solution in the peak area of dulolphol; 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 D 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 E requirements. 10% limit and recovery rate 10.1 Quantitation limits The quantitative limit of diclofenac in tea was 10 μg/kg, and the other substrates were 5 μg/kg. 10.2 Recovery rate For different substrates, the recovery rates for the three different additive levels are given in Appendix C. GB 23200.24-2016

Appendix A

(Informative) Reference mass spectrometry conditions 1) Reference mass spectrometry conditions. A) sheath gas pressure. 137.9 kPa (20 psi); B) Auxiliary gas pressure. 206.85 kPa (30 psi); C) Negative ion mode Electrospray voltage (IS). -3.200 V; D) Capillary temperature. 320 ° C; E) Source induced dissociation voltage. 10 V; F) Q1, Q3 resolution. Q1 is 0.4, Q3 is 0.7; G) collision gas. high purity argon; H) Collision gas pressure. 1.5 mTorr. I) Other mass spectral parameters are shown in Table A.1. Table A.1 Mass Spectral Acquisition Parameters and Retention Time Analyte retention time/min acquisition window/min ion pair (m/z) collision energy/eV Digoxin 4.55 3 ~ 6 239.02/194.05a 239.02/193.02 A for the quantitative ion pair, for different mass spectrometry equipment, instrument parameters may be different, before the determination of the mass spectrometry parameters should be optimized to the best. 1) Non-commercial declaration. The reference mass spectrometry conditions listed in Appendix B are performed on a Thermo TSQ Quantum Ultra AM-type LC/MS. The instrument type is for reference only and does not involve commercial purposes, and the standard user is encouraged to try different manufacturers or models. GB 23200.24-2016

Appendix B

(Informative) The multi-reaction monitoring quality chromatogram of dinol Diphenols Reference Substance Multi-Reaction Monitoring Mass Chromatogram, see Figure B.1. Figure B.1 Diphenols Reference Substance Multi-Reaction Monitoring Quality Chromatogram 239.02/193.02 239.02/194.05 GB 23200.24-2016

Appendix C

(Informative) Sample concentration and recovery of the experimental data Table C.1 Experimental data on the concentration and recovery of the sample Substrate addition level (μg/kg) Recovery% apple 5 76.4 ~ 94.8 10 72.2 ~ 85.6 50 86.9 ~ 100 Cabbage 5 72.7 to 92.4 10 79.8 to 98.4 50 84.3 ~ 100 Chestnut 5 77.2 ~ 95.6 10 75.4 to 94.9 50 79.6 ~ 95.6 beef 5 77.3 ~ 94.2 10 79.2 ~ 94.7 50 80.0 to 97.7 honey 5 76.3 ~ 91.4 10 77.5 ~ 94.2 50 79.5 ~ 95.0 wheat 5 74.9 ~ 96.5 10 78.2 ~ 94.1 50 81.1 to 99.8 chicken 5 77.4 ~ 91.0 10 76.1 to 97.4 50 82.8 ~ 94.8 5 81.1 to 91.3 10 79.2 ~ 101 50 82.5 to 99.3 Soybeans 5 76.2 ~ 97.8 10 85.8 ~ 102 50 86.8 ~ 100 milk 5 71.8 ~ 100 10 74.2 ~ 94.1 50 86.8 ~ 101 tea 10 87.4 ~ 102 50 84.7 ~ 101 100 89.9 ~ 100 GB 23200.24-2016

Appendix D

(Normative appendix) Laboratory repeatability requirements Table D.1 Laboratory repeatability requirements Measured component content Mg/kg Precision 0.001 36 > 0.01 > 1 14 GB 23200.24-2016

Appendix E

(Normative appendix) Inter-laboratory reproducibility requirements Table E.1 Inter-laboratory reproducibility requirements Measured component content Mg/kg Precision 0.001 54 > 0.01 > 1 19

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