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Delivery: <= 4 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.83-2016: Food safety national standard -- Detection Method of Net Residue of Different Rice Blast in Food Status: Valid
Basic dataStandard ID: GB 23200.83-2016 (GB23200.83-2016)Description (Translated English): Food safety national standard -- Detection Method of Net Residue of Different Rice Blast in Food Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 19,164 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 1967-2007 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.83-2016: Food safety national standard -- Detection Method of Net Residue of Different Rice Blast in Food---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 - Detection Method of Net Residue of Different Rice Blast in Food National standards for food safety Detection Method of Net Residue of Different Rice Blast in Food National food safety standards- Determination of iprobenfos residue in foods GB National Standards of People's Republic of China Instead of SN/T 1967-2007 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 ForewordThis standard replaces SN/T 1967-2007 "Method for the detection of residual rice residue in food for import and export". This standard and SN/T 1967-2007, the main changes are as follows. - Standard text format is modified to national standard text format for food safety; - the name and scope 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 1967-2007. National standards for food safety Detection Method of Net Residue of Different Rice Blast in Food1 ScopeThis standard specifies the method of gas chromatography-mass spectrometry for different rice blast in food. This standard applies to tea, spinach, buckwheat, apple, chestnut, honey, vinegar, rice, chicken, beef, fish, different rice Plague net residue determination and confirmation, other food can refer to the implementation.2 normative reference documentsThe following documents are indispensable for the application of this document. For dated references, only the date of the note applies This document. 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 methods3 method summaryThe residual rice blast in the sample was extracted with acetone and n-hexane (12), and the graphitized carbon black solid phase extraction column or neutral alumina Solid phase extraction column purification, elution concentrated and constant volume, the gas chromatography - mass spectrometer determination and confirmation, external standard quantitative.4 reagents and materialsUnless 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). Distillation. 4.1.2 Acetone (CH3COCH3). Distillation. 4.1.3 Sodium chloride (NaCl). 4.1.4 anhydrous sodium sulfate (Na2SO4). 650 ° C burning 4 h, set the dryer in the spare. 4.2 solution preparation 4.2.1 Acetone + n-Hexane (1 2) Solution. Take 100 mL of acetone, add.200 mL of n-hexane and shake well. 4.2.2 acetone + n-hexane (1 1) solution. take 100 mL of acetone, add 100 mL of n-hexane, shake back. 4.3 standards 4.3.1 Substituted rice blast standard substance (Iprobenfos, C13H21O3PS, CAS. 26087-47-8). purity > 99%. 4.4 standard solution preparation 4.4.1 standard reserve solution. accurately weighed the appropriate amount of different rice blast net standard material, with acetone will be formulated into 1000 μg/mL standard reserve Liquid, and then according to the test requirements with n-hexane diluted to the corresponding standard working solution. The standard solution is protected from light at 4ºC. 4.5 Materials 4.5.1 Graphitized carbon black solid phase extraction column. 3 mL, 125 mg, or equivalent. 4.5.2 Neutral Alumina Solid Phase Extraction Column. 3 mL, 125 mg, or equivalent.5 instruments and equipment5.1 Gas Chromatography-Mass Spectrometer, with electron bombardment ion source (EI source). 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Tissue crusher. 5.4 Scroll Mixer. 5.5 Solid phase extraction unit with vacuum pump. 5.6 multi-function micro-sample processor, or equivalent. 5.7 Low speed centrifuge. 3 000 r/min. 5.8 Centrifuge tube. 15 mL. 5.9 scale tube. 15 mL. 5.10 Microiner. 10 μL. 5.11 pulverizer.6 Preparation and storage of samples6.1 Preparation of the sample 6.1.1 Fruits or vegetables Take a representative sample 500 g, chopped water can not be washed, with a crusher to sample processed into a slurry. Mix well and put it clean Of the container, sealed and marked. 6.1.2 Tea and grain Take a representative sample of 500 g, crushed with a pulverizer and passed through a 2.0 mm round hole sieve. Mix well, into a clean sample container, Sealed and marked. 6.1.3 Meat and meat products Take a representative sample of 500 g, cut it, and use a crusher to process the sample into a slurry, mix it, and mix it into a clean sample Inside, sealed and marked. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Tea, bee products, condiments and cereals and other samples stored at 0 4 º C; fruits and vegetables and meat and meat products such as samples in - Frozen below 18ºC. During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue.7 Analysis steps7.1 Extraction For tea, chestnut, honey, rice samples, weighed 1 g homogeneous sample (accurate to 0.001 g), for spinach, buckwheat head, Apple, vinegar, chicken, beef, fish samples, weighed 2 g homogeneous sample (accurate to 0.001 g). Place the weighed sample at 15 mL Centrifuge tube, add 1 g of sodium chloride, add 2 mL of distilled water, mix on the mixer for 30 s, placed 15 min. Add 3 mL to C Ketone + n-hexane mixture, and mixed on a mixer for 2 min. 2500 r/min centrifugation 1 min, drawing the upper n-hexane extract in another A test tube. And then add 3 mL of acetone + n-hexane mixture to extract twice, the combined extract. 7.2 Purification 7.2.1 Tea, spinach, buckwheat head, apple, chestnut, honey sample A graphitized carbon black solid phase extraction column (1 cm high anhydrous sodium sulfate layer in the column) was installed in a solid phase extraction vacuum suction apparatus , First with 1 mL³3 acetone pre-elution extraction column, and then 1 mL³³ n-hexane pre-elution extraction column, discard all pre-eluent. will The n-hexane extract was added to the graphitized carbon black solid phase extraction column and the extract was completely eluted and then mixed with 3 mL of acetone + n-hexane The column was eluted and the flow rate was maintained at 1.5 mL/min. The whole effluent was collected and the nitrogen stream was blown to near dry at 45 ° C. Finally with positive Hexane volume to 0.5 mL for GC-MS analysis. 7.2.2 Vinegar, rice, chicken, beef, fish samples A neutral alumina solid phase extraction column (1 cm high anhydrous sodium sulfate layer in the column) was installed in a solid phase extraction vacuum suction apparatus On the first, with 3 mL of acetone pre-elution extraction column, and then 3 mL n-hexane pre-elution extraction column, discard all pre-leaching solution. A mixture of n-hexane The extract was added to a neutral alumina solid phase extraction column, and the extract was completely eluted and then eluted with 3 mL of an acetone + n-hexane mixture The column was collected and the flow rate was maintained at 1.5 mL/min. The whole effluent was collected and the nitrogen stream was blown to near dry at 45 ° C. Finally, with n-hexane capacity To 0.5 mL for GC-MS analysis. 7.3 Determination 7.3.1 Gas Chromatography - Mass Spectrometry Reference Conditions A) Column. HP-5MS quartz capillary column, 30 m 0.25 mm (id), film thickness 0.25 m, or equivalent; B) Column temperature. Initial temperature 80 ºC, rise to 205 ºC at 7 ºC/min and up to 280 ºC at 25 ºC/min 5 min; C) Inlet temperature. 280 ºC; D) Chromatography-Mass Spectrometer Interface Temperature. 270 ºC; E) Carrier gas. helium, purity greater than or equal to 99.995%, 0.8 mL/min; F) Injection volume. 1 μL; G) Injection method. no split injection, 1 min after the valve; H) ionization mode. EI; I) ionization energy. 70 eV; J) Detection method. Select the ion monitoring mode (SIM); K) monitoring ions (m/z). 203, 204, 246, 288; quantitative ions. 204; L) solvent delay. 10 min. 7.3.2 Determination and confirmation of chromatography According to the content of different rice blast in the sample solution, the standard working solution with similar peak area is selected, and the standard working fluid and sample solution The response value of the rice in the standard working solution and the sample solution should be within the linear range of the instrument detection. Under the same experimental conditions, the mass retention time of the material to be tested in the sample was the same as that of the standard working solution, After the sample quality chromatography, the selected ions are present, after comparing the abundance of the selected ions with the standard corresponding to the abundance of ions, Its value within the allowable range (allowable range in Table 1) can determine the existence of the corresponding sample in the sample. In the "7.3.1" provisions of this method Under the condition of chromatography, the reference retention time of the rice blast is 17.70 min, and the monitoring ion (m/z) abundance ratio is 203. 204. 246. 288 = 17. 100. 15. 19. See Appendix A for chromatograms and spectra. Table 1 Maximum qualitative error of relative ion abundance when qualitative gas chromatography-mass spectrometry 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 expressedUse the chromatographic data processor or calculate the content of isoflavone net in the sample according to the following formula (1). A ²Cs²V X = ------ (1) As ² m Where. X - the content of different rice blast in the sample, mg/kg, mg/kg; A - the peak area of the different rice blast in the sample solution; Cs - the standard working fluid in the concentration of different rice blast, micrograms per milliliter, μg/mL; As - the peak area of the different rice blast in the standard working fluid; V - the final volume of the sample solution, ml, mL; M - the amount of sample represented by the final sample, g, 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 precision9.1 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) Together with the requirements of Appendix C. 9.2 The ratio of the absolute difference between the two independent determinations obtained under reproducibility and its arithmetic mean (percentage) Together with the requirements of Appendix D. 10% limit and recovery rate 10.1 Quantitation limits The limit of the net limit of rice blast is 0.005 mg/kg. 10.2 Recovery rate When the levels were 0.005 mg/kg, 0.01 mg/kg, 0.02 mg/kg, the added recoveries of the different rice blast were given in Appendix B.Appendix A(Informative) Total Ion Flow Chromatogram and Mass Spectrometry of Purified Raw Material of 1 0. 01 01 .0 01 2 .0 01 3 .0 01 4 .0 01 5 .0 01 6 .0 01 7 .0 01 8 .0 01 9 .0 02 .0 02 1 .0 02 2. 0 02 3 .0 02 4 .0 0 T ime - - > A bundance (2 0 3 .7 0 to 2 0 4 .7 0). STD 0 9 0 5 D .D 1 7 .7 0 Figure A.1 Total ion chromatogram of the target substance of different rice blast 6 0 8 0 1 0 01 2 01 4 01 6 01 8 02 0 02 2 02 4 02 6 02 8 0 M/z - - > A bundance 0.20 97.5 119.0 tea 0.005 74.9 93.3 0.01 90.8 107.9 0.02 83.5 108.1 spinach 0.005 86.8110.1 0.01 91.9 110.5 0.02 107.1 118.9 apple 0.005 75.386.5 0.01 92.8 119.9 0.02 95.6 113.1 honey 0.005 96.8 114.4 0.01 97.7 115.5 0.02 91.2 112.8 Chestnut 0.005 109.9 120.9 0.01 90.2 108.8 0.02 88.8 119.5 Vinegar 0.005 93.4 104.2 0.01 89.9 100.6 0.02 95.2 107.2 Buckwheat head 0.005 87.698.5 0.01 93.7 100.6 0.02 82.1 94.3 Fish 0.005 81.8104.9 0.01 80.9 94.0 0.02 90.0 106.8 beef 0.005 86.499.4 0.01 92.4 111.0 0.02 94.2 111.9 chicken 0.005 70.9103.0 0.01 70.2 93.1 0.02 73.392.7Appendix C(Normative appendix) Laboratory repeatability requirements Table C.1 Laboratory repeatability requirements Measured component content Mg/kg Precision 0.001 36 > 0.01 > 1 14Appendix 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 Second, gas chromatography 11 Scope This standard specifies the method of gas chromatography for the determination of residual rice in rice. This standard applies to rice, spinach, apples, beef, chicken, fish, honey, chestnut, tea, vinegar and other foods in different rice Plague net residue determination, other food can refer to the implementation. 12 normative references The following documents are indispensable for the application of this document. For dated references, only the date of the note applies This document. 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 13 principle The residual rice blast in the sample was extracted with acetone + n-hexane (1 2) and n-hexane, and purified by solid phase extraction column. Flame photometric detector of the gas chromatograph for the determination of external standard method quantitative. 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. 14.1 Reagent 14.1.1 n-hexane (C6H14). re-distillation. 14.1.2 Acetone (CH3COCH3). Distillation. 14.1.3 anhydrous sodium sulfate (Na2SO4). 650 ° C burning 4 h, set the dryer in the spare. 14.2 solution preparation 14.2.1 acetone n-hexane (1 2) solution. take 100 mL of acetone, add.200 mL of n-hexane, shake back. 14.2.2 standard reserve solution. accurately weighed the appropriate amount of different rice blast net standard material, with acetone will be formulated into 1000 μg/mL standard reserve Liquid, and then according to the test requirements with n-hexane diluted to the corresponding standard working solution. The standard solution is protected from light at 4 ºC. 14.3 standards 14.3.1 Substituted rice blast standard substance (Iprobenfos, C13H21O3PS, CAS. 26087-47-8). purity > 99%. 14.4 Materials 14.4.1 Graphitized Carbon Black Solid Phase Extraction Column. 3 mL, 125 mg, or equivalent. 14.4.2 Neutral Alumina Solid Phase Extraction Column. 3 mL, 125 mg, or equivalent. 15 instruments and equipment 15.1 Gas Chromatograph. with Flame Photometric Detector (FPD). 15.2 Analysis of balance. 0.01 g and 0.0001 g. 15.3 Centrifuge. 3000 r/min. 15.4 multi-function micro-sample processor, or equivalent. 15.5 with a stopper centrifuge tube. 5 mL, 10 mL. 15.6 glass tube. 20 mL. 15.7 pointed mouth straw. 15.8 Micro adjustable pipettes. 10 μL,.200 μL, 1 000 μL. 15.9 Microinjector. 10 μL. 15.10 Quick Mixer. 16 Sample preparation and storage 16.1 Sample preparation 16.1.1 Fruits or vegetables Take a representative sample 500 g, chopped water can not be washed, with a crusher to sample processed into a slurry. Mix well and put it clean Of the container, sealed and marked. 16.1.2 Tea and Grains Take a representative sample of 500 g, crushed with a pulverizer and passed through a 2.0 mm round hole sieve. Mix well, into a clean sample container, Sealed and marked. 16.1.3 Meat and meat products After picking 500 g of the sample, it was chopped and the sample was processed into a slurry by a crusher and mixed into a clean sample container Inside, sealed and marked. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 16.2 Sample storage Tea, bee products, condiments and cereals and other samples stored at 0 4 ºC; fruits and vegetables and meat and meat products such as samples in - Frozen below 18ºC. During the operation of the sample preparation, the sample should be protected from contamination or changes in the content of the residue. 17 Analysis steps 17.1 Extraction and purification 17.1.1 For rice, chestnut, honey samples Weigh 2 g (accurate to 0.001 g) homogeneous sample in a 10 mL centrifuge tube, add 2 mL of water, add anhydrous sodium sulfate Of the saturated, add 2 mL of acetone + n-hexane mixture to extract twice, each 2 min, and then centrifuged 3 min (centrifugal speed 2 000 r/min), the upper layer of the extract was taken on the graduated centrifuge tube; the residue was extracted twice with 2 mL of n-hexane and the combined extracts were Centrifuge tube, in a multi-functional micro-sample processor or other equivalent equipment, at 40 ℃ with nitrogen flow to 1.0 mL, for Injection analysis. 17.1.2 For spinach, apples, vinegar samples Weigh 2 g (accurate to 0.001 g) homogeneous sample in a 10 mL centrifuge tube. For tea samples, weigh 0.5 g (exact to 0.001 g) homogeneous sample in a 10 mL centrifuge tube, add 2 mL of water, add anhydrous sodium sulfate to make it saturated with 2 mL of acetone + The mixture was extracted twice for 2 min each time and then centrifuged for 3 min (centrifugation at 2 000 r/min). Take the solution in another centrifuge tube. Residue and then 2 mL of n-hexane extraction twice, combined with the upper extract, to be purified. In graphitized carbon black The solid phase extraction column was charged with 1 cm high anhydrous sodium sulfate at the top of the solid phase extraction column. The solid phase extraction column was pre-eluted with 4 mL of acetone + n-hexane mixture To the whole pre-eluent, and then the above extract into the solid phase extraction column, all the extract to the solid phase extraction column, and then 4 mL Acetone + n-hexane mixture to collect all the effluent in a graduated centrifuge tube, and finally in the multi-functional micro-sample processor or its He was on a comparable instrument and was blown to 1.0 mL at 40 ° C with a nitrogen stream for sample analysis. 17.1.3 For beef, chicken, fish samples Weigh 2 g (accurate to 0.001 g) homogeneous sample in 10 mL centrifuge tube, add anhydrous sodium sulfate to make it saturated, with 6 mL Acetone + n-hexane mixture was extracted once for 2 min, then centrifuged for 3 min (centrifugation speed of 2 000 r/min) Set the upper extract in another tube. Residue and then 2 mL of n-hexane extraction twice, combined with the upper extract, to be purified. In neutral oxygen The solid phase extraction column was packed with 1 cm high anhydrous sodium sulfate at the top of the aluminum solid phase extraction column. The solid phase extraction column was pre-leached with 4 mL of acetone + n- Discard all the pre-leaching solution, and then the extract into the solid phase extraction column, all the extract to the soli......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 23200.83-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.83-2016_English as soon as possible, and keep you informed of the progress. The lead time is typically 2 ~ 4 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of GB 23200.83-2016_English with my colleagues?Answer: Yes. 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