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GB 23200.89-2016 English PDF

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GB 23200.89-2016: Food safety national standard -- Determination of ethoxyquinoline residues in animal-derived foods by liquid chromatography
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GB 23200.89-2016English259 Add to Cart 3 days [Need to translate] Food safety national standard -- Determination of ethoxyquinoline residues in animal-derived foods by liquid chromatography Valid GB 23200.89-2016

PDF similar to GB 23200.89-2016


Standard similar to GB 23200.89-2016

GB/T 38211   GB/T 18418   GB/T 18419   GB 23200.82   GB 23200.83   GB 23200.81   

Basic data

Standard ID GB 23200.89-2016 (GB23200.89-2016)
Description (Translated English) Food safety national standard -- Determination of ethoxyquinoline residues in animal-derived foods by liquid chromatography
Sector / Industry National Standard
Classification of Chinese Standard G25
Word Count Estimation 13,181
Date of Issue 2016-12-18
Date of Implementation 2017-06-18
Older Standard (superseded by this standard) SN/T 2539-2010
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 23200.89-2016: Food safety national standard -- Determination of ethoxyquinoline residues in animal-derived foods by liquid chromatography


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Food safety national standard - Determination of ethoxyquinoline residues in animal - derived foods by liquid chromatography Replace SN/T 2539-2010 National Standards of People's Republic of China GB National standards for food safety Determination of the Residual Amount of Ethoxyquinoline in Animal - derived Food Liquid chromatography National food safety standards- Determination of ethoxyquin residue in animal-derived foods Liquid chromatography 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 2539-2010 "Determination of ethoxylated quinoline residues in animal food by high performance liquid chromatography". Compared with SN/T 2539-2010, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN/T 2539-2010. National standards for food safety Determination of ethoxyquinoline residues in animal - derived foods by liquid chromatography

1 Scope

This standard specifies the pork, pig liver, pig kidney, chicken, fish, eggs, honey, milk, ethoxyquinoline residues in liquid chromatography Determination and determination of high performance liquid chromatography - mass spectrometry. This standard is applicable to the determination and determination of ethoxyquinoline residues in pork, pig liver, pig kidney, chicken, fish, eggs, honey and milk. Card, 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 file. 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

After the sample was added with sodium carbonate solution and extracted with acetone, the liquid-liquid extraction was carried out with n-hexane. After the solution was concentrated and concentrated, With high performance liquid chromatography with high performance liquid chromatography - tandem mass spectrometer, quantitative 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 Acetone (C3H6O, 67-64-1). Chromatographic pure. 4.1.2 n-hexane (C6H14,110-54-3). chromatographic purity. 4.1.3 acetonitrile (C2H3N, 75-05-8). pure chromatography. 4.1.4 Sodium carbonate (Na2CO3, 497-19-8). 4.1.5 Ammonium Acetate (C2H7NO2,631-61-8). Chromatographic Purification. 4.2 solution preparation 4.2.1 sodium carbonate solution (10%). accurately weighed 100 g of sodium carbonate in the beaker by adding the appropriate amount of water dissolved, transferred to 1L volumetric flask, constant volume To the scale, shake. 4.2.2 ammonium acetate solution (20mmol/L). accurately weighed 1.54 g ammonium acetate, dissolved in 1L water. 4.3 standards 4.3.1 ethoxyquinoline standard substance (C14H19NO, 91-53-2). purity ≥ 98.0%. 4.4 standard solution preparation 4.4.1 ethoxyquinoline standard stock solution. accurately weighed the amount of standard, diluted with acetonitrile prepared 100 μg/mL standard stock solution, In 0 ℃ ~ 4 ℃ dark preservation. 4.3.2 ethoxyquinoline standard working solution. according to the need to remove a certain volume of standard intermediate solution with acetonitrile gradually diluted to the appropriate concentration Of the standard working solution. Standard working solution is ready for use.

5 instruments and equipment

5.1 High Performance Liquid Chromatograph. equipped with a fluorescence detector (FLD). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 High Performance Liquid Chromatography-Tandem Mass Spectrometer with Electrospray Ionization Source (ESI). 5.4 Tissue crusher. 5.5 Centrifuge. 6 000 r/min. 5.6 Scroll Mixer. 5.7 Rotary Evaporator. 5.8 Analytical balance. sensed 0.0001 g and 0.01 g. 5.9 nitrogen blowing concentrator. 5.10 Organic filter. 0.22 μm.

6 Preparation and storage of samples

6.1 Preparation of the sample 6.1.1 Meat and internal organs Take a representative sample 500 g, cut it, and then use the tissue crusher to process the sample into a slurry, mix it, and mix it into a clean sample Inside, sealed and marked. 6.1.2 honey and milk Take a representative sample of 500 g, pour it into a clean enamel mix bucket, stir well and mix it into a clean container. And mark the mark. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Milk, honey samples stored at 0 ℃ ~ 4 ℃; meat and visceral products such as samples at -18 ℃ frozen storage. During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue.

7 Analysis steps

7.1 Extraction Weigh 2 g homogeneous sample (accurate to 0.01 g) in a 50 mL stoppered centrifuge tube and add 5 mL of sodium carbonate solution to the vortex Mix for 5 minutes, add 5 mL of acetone to the vortex mixer for 2 min, add 15 mL of n-hexane, in the vortex mixer Extraction of 2 min, 6000 r/min centrifugation 3min, take the upper layer of n-hexane in.200 mL chicken heart bottle, with 15 mL n-hexane and then repeat Take the n-hexane layer in the heart of the heart, and extract the extract to a concentration of about 1 mL in a 30 ° C water bath and blow it with a gentle nitrogen stream Close to dry, dissolved in acetonitrile and set to 1.0 mL, filter membrane, for high performance liquid chromatography and high performance liquid chromatography - tandem mass spectrometry Confirmation. 7.2 Determination 7.2.1 Reference conditions for high performance liquid chromatography A) Column. C18, 150 mm x 4.6 mm (inner diameter), 5 μm, or equivalent; B) Column temperature. 25 ° C; C) mobile phase. ammonium acetate aqueous solution (20 mmol/L) acetonitrile = (7 3, V/V); D) Fluorescence detector. excitation wavelength 360nm, emission wavelength 435nm; E) Flow rate. 0.50 mL/min; F) Injection volume. 10 μL. 7.2.2 High Performance Liquid Chromatography - Tandem Mass Spectrometer Determination of Reference Conditions 7.2.2.1 High Performance Liquid Chromatography Reference Conditions A) Column. C18, 150 mm × 4.6 mm (inner diameter), 5 μm or equivalent. B) Column temperature. 25 ° C; C) Flow rate. 0.50 mL/min; D) gradient elution procedure. see Table 1; E) Injection volume. 5 μL. Table 1 High Performance Liquid Chromatography - Tandem Mass Spectrometer Gradient Elution Procedure Time/min flow rate/(mLmin) 5 mmol/L ammonium acetate aqueous solution /% acetonitrile /% 0 0.5 60 40 3 0.5 40 60 6 0.5 10 90 9 0.5 10 90 11 0.5 60 40 14 0.5 40 60 7.2.2.2 Mass spectrometry reference conditions See Appendix A for reference conditions. 7.2.3 Determination by high performance liquid chromatography According to the content of ethoxyquinoline in the sample solution, the standard working solution of ethoxyquinoline with similar concentration was selected. Standard working solution and sample solution The response value of ethoxyquinoline should be within the linear range of the instrument. On the standard working fluid and sample volume of alternating injection to determine the volume Time to qualitative, measured sample solution with the standard working fluid peak area compared to quantitative. In the above high performance liquid chromatography conditions, ethoxyquinoline standards See Figure B.1 for chromatograms. 7.2.3.1 High performance liquid chromatography - tandem mass spectrometry If the retention time of the detected peaks is consistent with the standard sample, the mass of the sample is determined by the mass spectrometry. certificate. When the sample was confirmed by high performance liquid chromatography-tandem mass spectrometry, the relative abundance of each qualitative ion And the concentration of close to the same conditions obtained under the standard solution spectrum comparison. Under the same experimental conditions, the mass of the test substance in the sample solution The peak retention time is consistent with that in the standard solution, and the selected qualitative ions are present, and the relative abundance of the selected qualitative ions is the same as that of the standard sample Of the relative abundance of uniform (allowable deviation range in Table 2), you can determine the existence of the corresponding sample in the sample. If you can not confirm, you should re-enter , With a scanning method (with sufficient sensitivity) or by adding other confirmed ions or with other higher sensitivity analytical instruments certificate. In the above-mentioned high performance liquid chromatography-tandem mass spectrometry conditions, the selective ion monitoring chromatogram of the ethoxyquinoline standard is shown in Figure C.1. Table 2 The maximum allowable deviation 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% 7.3 blank test In addition to the sample, according to the above determination steps.

8 results are calculated and expressed

Use the chromatographic data processor or calculate the residual content of ethoxyquinoline in the sample according to formula (1). The calculation result is deducted from the blank value. MA VCA  (1) Where. X - Residual content of ethoxyquinoline in milligrams per kilogram (mg/kg); A - the peak area of ethoxyquinoline in the sample solution; SC - Concentration of ethoxyquinoline in standard working solution in micrograms per milliliter (μg/mL); V - Final volume of volume in milliliters (mL); SA - peak area of ethoxyquinoline in standard working solution; M - the mass of the sample represented by the final sample, in grams (g). Note. The result of the calculation should be deducted from the blank value. The result of the measurement is expressed by the arithmetic mean of the parallel measurement, and the two valid digits are retained. When the result is greater than 1 mg/kg Retain three valid digits.

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 the requirements of E. 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 F requirements. 10% limit and recovery rate 10.1 Quantitation limits The method of quantification of ethoxyquinoline is 0.01 mg/kg. 10.2 Recovery rate When the levels were 0.01 mg/kg, 0.05 mg/kg, 0.1 mg/kg, the addition of ethoxyquinoline in different substrates was See Appendix D.

Appendix A

(Informative) Mass spectrometry conditions A.1 Mass spectrometry conditions are given in Table A.1 Table A.1 Mass spectrometry conditions Ion source electrospray ionization ionization source (ESI), positive ion monitoring Scan mode selection Ion monitoring (SRM) Air Curtain (CUR) 68.95 kPa (10 psi) Atomization gas (GS1) 275.8 kPa (40 psi) Auxiliary heating gas (GS2) 344.75 kPa (50 psi) Collision gas (CAD) 48.27 kPa (7 psi) Electromagnetic spray voltage (IS) 5 000 V Ion source temperature (TEM) 450 ° C A.2 Select the ion monitoring conditions shown in Table A.2 Table A.2 Select the ion monitoring conditions To be measured Q1 M/z Q3 M/z To cluster voltage DP/V Collision voltage CE/V Collision chamber chamber voltage EP/V The chamber voltage of the collision chamber CXP/V Ethoxyquinoline 218.1 148.1a 74 31 10 12 190.4 74 30 10 6 202.1 74 28 10 9 Note. "a" is a quantitative ion pair 1) Non-commercial notices. The parameters listed in Appendix A are done on the API4000 mass spectrometer. The test instrument model listed here is for reference only and does not Involving commercial purposes, to encourage standard users to try to use different manufacturers or models of equipment.

Appendix B

(Informative) Ethoxyquinoline standard liquid chromatography B.1 Ethoxyquinoline standard liquid chromatogram shown in Figure B.1 Min0 2.5 5 7.5 10 12.5 LU Gt; 0. Figure B.1 Ethoxyquinoline standard (0.2 mg/kg) Liquid chromatogram

Appendix C

(Informative) Ethoxyquinoline standard selection ion monitoring (SRM) chromatogram C.1 Ethoxyquinoline Standard Selective Ion Monitoring (SRM) Chromatogram See Figure C.1 Figure C.1 Ethoxyquinoline standard (0.02 mg/kg) Select ion monitoring (SRM) chromatogram 1 2 3 4 5 6 7 8 9 10 11 12 13 0.0 2.0e4 4.0e4 4.8e4 10.28 1 2 3 4 5 6 7 8 9 10 11 12 13 0.0 2.0e4 4.0e4 4.8e4 10.28 1 2 3 4 5 6 7 8 9 10 11 12 13 T/min 0.0 1.0e4 2.0e4 3.0e4 3.7e4 10.28 1 2 3 4 5 6 7 8 9 10 11 12 13 0.0 1.0e4 2.0e4 2.8e4 10.28 TIC 218.1 > 148.1 218.1 > 190.41 218.1 > 202.1 T/min T/min

Appendix D

(Informative) The recovery of ethoxyquinoline in different sample substrates D.1 Recovery of ethoxyquinoline in different sample substrates is shown in Table D.1 Table D.1 Recovery of ethoxyquinoline in different sample substrates Sample Substrate Add Concentration/(mg/kg) Recovery /% Sample Substrate Add Concentration/(mg/kg) Recovery /% pork 0.01 89.5 108.0 honey 0.01 89.2  100.3 0.05 84.2  102.2 0.05 88.8  101.2 0.10 86.898.2 0.10 84.190.5 Liver 0.01 92.7  109.0 egg 0.01 90.3  101.4 0.05 93.2  109.2 0.05 93.7  107.5 0.1 90.6 98.4 0.10 96.6  101.6 Pig kidney 0.01 85.8  102.0 Fish 0.01 94.7  102.1 0.05 91.3 105.6 0.05 87.7 108.0 0.10 92.0105.6 0.10 92.097.7 chicken 0.01 84.8  101.1 milk 0.01 91.41010.1 0.05 85.8  102.6 0.05 83.9  95.2 0.10 86.199.5 0.10 87.489.8

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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