GB 23200.105-2016 English PDFUS$219.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email. GB 23200.105-2016: Food safety national standard -- Meat and meat products -- Determination of carbazate residues -- Liquid chromatography -- Post-column derivatization fluorescence detection Status: Valid
Basic dataStandard ID: GB 23200.105-2016 (GB23200.105-2016)Description (Translated English): Food safety national standard -- Meat and meat products -- Determination of carbazate residues -- Liquid chromatography -- Post-column derivatization fluorescence detection Sector / Industry: National Standard Classification of Chinese Standard: G25 Word Count Estimation: 11,161 Date of Issue: 2016-12-18 Date of Implementation: 2017-06-18 Older Standard (superseded by this standard): SN/T 0122-2011 Regulation (derived from): State Health Commission, Ministry of Agriculture, Food and Drug Administration Notice No. 16 of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 23200.105-2016: Food safety national standard -- Meat and meat products -- Determination of carbazate residues -- Liquid chromatography -- Post-column derivatization fluorescence detection---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 - Meat and meat products - Determination of carbazate residues - Liquid chromatography - post - column derivatization fluorescence detection National Standard of the People 's Republic of China GB 0521-200 National standards for food safety Determination of Carnosilvine Residue in Meat and Meat Products Liquid Chromatography - Post - column Derivative Fluorescence Detection National food safety standards- Determination of carbaryl residue in meat and meat products HPLC-fluoresce detector with post column derivation 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 Instead of SN/T 0122-2011 ForewordThis standard replaces SN/T 0122-2011 "Determination of Carbendazim Residue in Import and Export Meat and Meat Products Liquid Chromatography - Post-column Derived Fluorescence Light detection method ". Compared with SN/T 0122-2011, 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 of meat and meat products" to "meat and meat products"; - increase the "other food reference implementation" in the standard range. This standard replaced the previous version of the standard release. -SN 0122-1992; -SN/T 0122-2011. National standards for food safety Determination of Carnosilvine Residue in Meat and Meat Products Liquid Chromatography - Post - column Derivative Fluorescence Detection1 ScopeThis standard specifies the liquid and liquid chromatography-post-column derivatization fluorescence detection method for the removal of carbaryl residues in meat and meat products. This standard applies to the import and export of beef, chicken, shrimp, fish and ham in the determination of the residual amount of decamethrin, other food can refer to carried out.2 normative reference documentsThe 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 2763-2014 National Standard for Food Safety - Maximum Residue Limits for Pesticides in Foodstuffs Analysis of laboratory water specifications and test methods GB/T 6682-20083 principleThe residue of the decamethrin in the sample was extracted with a mixture of acetone and petroleum ether. After purification by gel column, the mixture was concentrated and analyzed by high performance liquid chromatography Separation, after column derivatization, with the fluorescence detector detection, external standard quantitative.4 reagents and materialsUnless otherwise specified, all reagents are analytical reagent and water is a Class I water specified in GB/T 6682. 4.1 Reagents 4.1.1 Acetonitrile (CH3CN). Chromatographically pure. 4.1.2 Ethyl acetate (C4H8O2). Chromatographic purity. 4.1.3 Cyclohexane (C6H12). Chromatographic Purification. 4.1.4 Acetone (CH3COCH3). Chromatographic pure. 4.1.5 petroleum ether. boiling range 30 ℃ ~ 60 ℃. 4.1.6 anhydrous sodium sulfate (Na2SO4). 650 ℃ burning 4 h, in the dryer to cool to room temperature, stored in a sealed bottle in reserve. 4.1.7 Sodium chloride (NaCl). 4.1.8 post-column derivatization reagents. 4.1.9 o-phthalaldehyde (C8H602, O-Phthaladehyde, OPA). 4.1.10 mercaptoethanol (C2H6OS, Thiofluor). 4.2 solution preparation 4.2.1 NaOH solution (0.2%, m/v). take 2 g NaOH, the volume of water to 1000 mL. 4.2.2 O-phthalaldehyde diluent. borax solution (0.4%, m/v). 4.2.3 O-phthalaldehyde test solution. 945 ml of OPA diluent was injected into the solvent tank and purged with inert gas (nitrogen) for at least 10 min, 100 mg of OPA solids were dissolved in about 10 mL of chromatographic pure methanol and the OPA solution was added to the deoxygenated OPA diluent to dissolve 2 g of mercaptan Base ethanol solids in 5 mL OPA diluent, added to the tank, covered with cap, open airflow, and then continue to purge for a few minutes, The valve is gently agitated to make it completely mixed. 4.2.4 Ethyl acetate-cyclohexane mixed solution (1 1, v/v). Take 100 mL of ethyl acetate, add 100 mL of cyclohexane and shake well. 4.3 standards 4.3.1 Carbaryl. Molecular formula C12H11NO2, CAS 63-25-2, purity > 99.5%. 4.4 standard solution preparation 4.4.1 Monazalose standard stock solution. accurately weighed the right amount of methacon standard, dissolved in acetonitrile, 4 ℃ refrigerator, valid for 6 month. Store in 4 ℃ refrigerator. 4.4.2 Carbaryl standard working solution. take a certain amount of standard stock solution, diluted with acetonitrile to the appropriate concentration, 4 ℃ refrigerator, valid for 1 week. Store in 4 ℃ refrigerator. 4.5 Materials 4.5.1 0.45 μm nylon filter.5 instruments and equipment5.1 Liquid Chromatography. equipped with fluorescence detectors and post-column derived units. 5.2 Analysis of balance. 0.01 g and 0.0001 g. 5.3 Fully automatic gel chromatograph (with fraction collection concentrator). 5.4 Rotary Evaporator. 5.5 nitrogen blowing instrument. 5.6 Tissue homogenizer. 5.7 Oscillator.6 Preparation and storage of samples6.1 Preparation of the sample 6.1.1 meat All the samples taken, fully mixed and mixed, take a representative sample, the total amount of not less than 500 g, into the cleaning container, sealed And mark the mark. 6.1.2 canned The whole sample of the whole pot can be poured out, fully blended mix, take a representative sample, the total amount of not less than 500 g, into the cleaning container Sealed and marked. Note. The above sample sampling site according to GB 2763 Appendix A implementation. 6.2 Sample storage Samples should be stored below -18 ° C. In the operation of sampling and sample preparation, the sample should be protected from contamination or changes in content. The test sample can represent the overall sample.7 Analysis steps7.1 Extraction Weigh the sample 20 g (accurate to 0.01 g), add 100 mL of water in a 100 mL stopper, add water 6 mL (depending on the moisture content of the sample Water about 20 g, meat is usually about 70%, add water 6 mL), add 40 mL of acetone, homogenate 1 min, add sodium chloride 6 g, shake well, Plus 30 mL of petroleum ether, shake for 30 min. Take 35 mL of the organic layer supernatant, filtered through anhydrous sodium sulfate in a rotary vial and concentrated to About 1 mL, add 2 mL of ethyl acetate-cyclohexane solution and re-concentrate, so repeat 3 times. Ethyl acetate - cyclohexane volume of 5 mL, 0.45 μ M filter filter, to be purified. 7.2 Gel Chromatography (GPC) purification 7.2.1 Gel Chromatographic Purification Reference Conditions A) Purification column. 400 mm × 30 mm, Bio Beads S-X3, or equivalent. B) Mobile phase. ethyl acetate-cyclohexane. C) Flow rate. 5.0 mL/min. D) Sample loop. 5 mL. E) Distillate collection section. 10.0 min ~ 15.0 min. F) purification column balance time. 5 min. 7.2.2 Gel Chromatography Concentration Reference conditions A) Sample concentration conditions are shown in Table 1. B) Concentration end point determination. Level sensing mode. C) Solvent Replacement. 2 mL acetonitrile, repeated twice. D) constant volume. 1 mL. 7.2.3 Gel Chromatography Purification Procedure 5 mL of the purified liquid according to the conditions specified in 7.2.1 and 7.2.2 purification and concentration, and finally get 1 mL of the solution to be determined. Table 1 Fraction Concentration Conditions Concentration Period Concentration Cup Area Temperature (° C) Vacuum (Torr) Sample concentration process Zone 1 50 280 Zone 2 52 220 Zone 3 54 Concentration end point arrival process Zone 1 52 220 Zone 2 53 220 7.3 Determination 7.3.1 Liquid Chromatographic Reference Conditions A) Column. C18,250 mm x 4.6 mm x 5 μm, or equivalent; B) Column temperature. 42 ° C; C) Fluorescence detector. λex 330 nm, λem 465 nm; D) mobile phase. acetonitrile water (40 60, volume ratio); E) Flow rate. 1.0 mL/min; F) Injection volume. 20 L. 7.3.2 post-column derivatization A) Derivative reagent 1. Hydrolysis reagent, 0.4% sodium hydroxide solution, flow rate 0.4 mL/min; B) Derivative reagent 2. OPA reagent at a flow rate of 0.4 mL/min; C) Reactor temperature. hydrolysis temperature is 100 ° C and the temperature is room temperature. 7.3.3 Chromatographic determination According to the content of kaempferol measured in the sample solution, the standard working fluid with similar concentration should be selected. The response value should be in the linear range Inside. Under the above liquid chromatographic conditions, the retention time of Carbaryl is 11.1 min, and the chromatogram is shown in Figure A.1 in Appendix A. 7.3.4 Blank test In addition to the sample, according to the above steps.8 results are calculated and expressedAccording to formula (1) to calculate the content of carnosilane in the sample. MA VCA (1) Where. X - The amount of carbaryl in the sample, in milligrams per kilogram (mg/kg); A - the chromatographic peak area of carbaryl in the sample; Cs - the concentration of carbaryl in the standard working solution in micrograms per milliliter (μg/mL); V - the final volume of the sample solution in milliliters (mL); As - the chromatographic peak area of carbamate in standard working solution; M - the amount of the final sample, expressed 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 precision9.1 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, recovery rate 10.1 Quantitation limits The limit of quantification of this method is 0.005 mg/kg. 10.2 Recovery rate The recovery rate of norethium is shown in Appendix B.Appendix A(Informative) Monochloride standard chromatogram Figure A.1 Liquid Chromatography (0.1 μg/mL)Appendix B(Informative) Sample concentration and recovery of the experimental data Table B.1 Experimental data on the concentration and recovery of the sample sample Add level (Mg/kg) Recovery rate range (%) sample Add level (Mg/kg) Recovery rate range (%) Fish 0.005 82.0 ~ 110.0 Ham 0.005 90.0 to 96.0 0.010 89.0 to 107.0 0.010 100.0 to 114.0 0.020 94.0 to 112.5 0.020 97.0 to 115.5 0.050 90.0 to 105.6 0.050 101.6 to 113.6 0.100 92.0 to 111.2 0.100 92.5 to 107.3 beef 0.005 82.0 ~ 98.0 Shrimp 0.005 86.0 ~ 100.0 0.010 86.0 to 99.0 0.010 85.0 to 96.0 0.020 84.5 to 109.5 0.020 87.0 to 105.0 0.050 90.6 ~ 98.0 0.050 88.6 ~ 94.6 0.100 88.4 ~ 98.0 0.100 86.7 ~ 95.1 chicken 0.005 86.0 to 96.0 0.010 89.0 to 97.0 0.020 95.5 to 112.5 0.050 92.0 to 97.2 0.100 85.9 ~ 95.0 5.000 87.7 to 102.5Appendix 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 ......Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of GB 23200.105-2016_English be delivered?Answer: Upon your order, we will start to translate GB 23200.105-2016_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time.Question 2: Can I share the purchased PDF of GB 23200.105-2016_English with my colleagues?Answer: Yes. The purchased PDF of GB 23200.105-2016_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet.Question 3: Does the price include tax/VAT?Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countriesQuestion 4: Do you accept my currency other than USD?Answer: Yes. If you need your currency to be printed on the invoice, please write an email to Sales@ChineseStandard.net. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay. |
