GB 5009.22-2016 PDF EnglishUS$245.00 · In stock · Download in 9 seconds
GB 5009.22-2016: National food safety standard - B-group and G-group aflatoxins in foods Delivery: 9 seconds. True-PDF full-copy in English & invoice will be downloaded + auto-delivered via email. See step-by-step procedure Status: Valid GB 5009.22: Historical versions
Similar standardsGB 5009.22-2016: National food safety standard - B-group and G-group aflatoxins in foods---This is an excerpt. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.), auto-downloaded/delivered in 9 seconds, can be purchased online: https://www.ChineseStandard.net/PDF.aspx/GB5009.22-2016GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA National Food Safety Standard - Determination of B- group and G-group Aflatoxins in Foods Issued on. DECEMBER 23, 2016 Implemented on. JUNE 23, 2017 Issued by. National Health and Family Planning Commission of the PRC; China Food and Drug Administration. Table of ContentsForeword... 4 1 Scope... 5 2 Principle... 6 3 Reagents and materials... 6 4 Instruments and equipment... 8 5 Analytical procedures... 9 6 Expression of analytical results... 15 7 Precision... 15 8 Others... 16 9 Principle... 16 10 Reagents and materials... 16 11 Instruments and equipment... 18 12 Analytical procedures... 19 13 Expression of analytical results... 21 14 Precision... 22 15 Others... 22 16 Principle... 23 17 Reagents and materials... 23 18 Instruments and equipment... 25 19 Analytical procedures... 27 20 Expression of analytical results... 31 21 Precision... 32 22 Others... 32 23 Principle... 33 24 Reagents and materials... 33 25 Instruments and equipment... 33 26 Analytical procedures... 34 27 Expression of analytical results... 34 28 Precision... 35 29 Others... 35 30 Principle... 36 31 Reagents and materials... 36 32 Instruments and equipment... 38 33 Analytical steps... 38 34 Precision... 46 35 Others... 46 Appendix A Calibration method of standard concentration of AFT B1, AFT B2, AFT G1 and AFT G2... 47 Appendix B Method of verification of immunoaffinity column... 49 Appendix C Tandem mass spectrometry... 50 Appendix D Liquid chromatogram... 55 Appendix E Determination method of quality of enzyme-linked immunosorbent kit... 591 ScopeThis standard specifies the method for determination of aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2 (hereinafter referred to as AFT B1, AFT B2, AFT G1 and AFT G2) in food. The first method of this standard is the isotope dilution liquid chromatography- tandem mass spectrometry, which is suitable for the determination of AFT B1, AFT B2, AFT G1 and AFT G2 in cereals and their products, beans and their products, nuts and seeds, fats and their products, seasonings, infant formula and infant complementary foods. The second method of this standard is the high-performance liquid chromatography-pre-column derivatization, which is suitable for the determination of AFT B1, AFT B2, AFT G1 and AFT G2 in cereals and their products, beans and their products, nuts and seeds, fats and their products, seasonings, infant formula and infant complementary foods. The third method of this standard is the high-performance liquid chromatography-post-column derivatization, which is suitable for the determination of AFT B1, AFT B2, AFT G1 and AFT G2 in cereals and their products, beans and their products, nuts and seeds, fats and their products, seasonings, infant formula and infant complementary foods. The fourth method of this standard is the enzyme-linked immunoadsorption screening method, which is suitable for the determination of AFT B1 in cereals and their products, beans and their products, nuts and seeds, fats and their products, seasonings, infant formula and infant complementary foods. The fifth method of this standard is the thin-layer chromatography, which is suitable for the determination of AFT B1 in cereals and their products, beans and their products, nuts and seeds, fats and their products, and seasonings. Method I. Isotope dilution liquid chromatography- tandem mass spectrometry2 PrincipleThe aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2 in the specimen are extracted by acetonitrile-water solution or methanol-water solution. After the extract is diluted by the phosphate buffer solution which contains 1% Triton X- 100 (or Tween-20) (if necessary, it is initially purified by the aflatoxin solid-phase purification column), through purification and enrichment by immunoaffinity column, the purification liquid is concentrated, constant-volume, filtered, separated by liquid chromatography, tested by tandem mass spectrometry, then subjected to quantification by isotope internal standard method.3 Reagents and materialsUnless otherwise stated, the reagents used in this method are of analytical grade, the water is the grade I water as specified in GB/T 6682. 3.1 Reagents 3.2 Preparation of reagents 3.3 Standard substance 3.3.1 AFT B1 standard substance (C17H12O6, CAS. 1162-65-8). Purity ≥ 98%, or 3.4 Preparation of standard solution4 Instruments and equipment4.1 Homogenizer. 4.2 High-speed pulverizer. 4.3 Tissue masher. 4.4 Ultrasonic / vortex oscillator or shaker. 4.5 Balance. Sensitivity is 0.01 g and 0.00001 g. 4.6 Vortex mixer. 4.9 Glass-fiber filter paper. Fast, high-load, which retains 1.6 μm particles in liquid. 4.13 Liquid chromatography column. 4.14 Immunoaffinity column. Capacity of AFT B1 column ≥ 200 ng, recovery rate of AFT B1 column ≥ 80%, cross-reaction rate of AFT G2 ≥ 80% (see Appendix B for verification method). 4.15 Aflatoxin-specific solid-phase extraction purification column or functionally equivalent solid-phase extraction column (hereinafter referred to as purification column). which is used for the determination of samples of complex matrix. 4.18 pH meter.5 Analytical proceduresThe use of immunoaffinity columns from different manufacturers may slightly differ in sample loading, rinsing and elution operations, so it shall be performed in accordance with the operation instructions as provided by the manufacturer. Caution. 5.1 Preparation of sample 5.1.1 Liquid samples (vegetable oil, soy sauce, vinegar, etc.) The sampling amount shall be greater than 1 L. For packaging samples such as bags and bottles, it shall collect at least 3 packages (same batch or number). All liquid samples shall be mixed by a homogenizer in a container, any 100 g (mL) of sample is taken for testing. 5.1.2 Solid samples (cereals and their products, nuts and seeds, cereal supplements for infants, etc.) The sampling amount shall be greater than 1 kg. It shall be crushed by high- speed pulverizer and sieved to make the particle size less than the 2 mm aperture test sieve. It is evenly mixed and then reduced to 100 g, stored in the sample bottle, sealed for preservation, to prepare for testing. 5.1.3 Semi-fluid (fermented bean curd, fermented soybean, etc.) The sampling amount shall be greater than 1 kg (L). For packaging samples such as bags and bottles, it shall collect at least 3 packages (same batch or number). Then it is crushed and mixed uniformly by the tissue crusher, stored in sample bottle, sealed for preservation, to prepare for testing. 5.2 Extraction of sample 5.2.1 Liquid sample 5.2.2 Solid sample 5.2.2.1 General solid samples WEIGH 5 g of specimen (accurate to 0.01 g) into a 50 mL centrifuge tube; ADD 100 μL of isotope internal standard working solution; OSCILLATE to mix it; LET it be standing for 30 min. ADD 20.0 mL of acetonitrile-water solution (84 + 16) or methanol-water solution (70 + 30); VORTEX to mix it uniformly; PLACE it in the ultrasonic/vortex oscillator or shaker to oscillate it for 20 min (or homogenized by homogenizer for 3 min) 5.2.2.2 Infant formula and infant complementary foods WEIGH 5 g of specimen (accurate to 0.01 g) into a 50 mL centrifuge tube; ADD 100 μL of isotope internal standard working solution; OSCILLATE to mix it; LET it be standing for 30 min. ADD 20.0 mL of acetonitrile-water solution (50 + 50) or methanol-water solution (70 + 30); VORTEX to mix it uniformly; PLACE it in the ultrasonic/vortex oscillator or shaker to oscillate it for 20 min (or homogenized by homogenizer for 3 min). 5.2.3 Semi-fluid sample WEIGH 5 g of specimen (accurate to 0.01 g) into a 50 mL centrifuge tube; ADD 100 μL of isotope internal standard working solution; OSCILLATE to mix it; LET it be standing for 30 min. ADD 20.0 mL of acetonitrile-water solution (84 + 16) or methanol-water solution (70 + 30); PLACE it in the ultrasonic/vortex oscillator or shaker to oscillate it for 20 min (or homogenized by homogenizer for 3 min). CENTRIFUGE it at 6000 r/min for 10 min (or otherwise homogenized and then filtered by glass-fiber filter paper), TAKE the supernatant to prepare for use. 5.3 Purification of sample 5.3.1 Purification of immunoaffinity column 5.3.2 Simultaneous use of aflatoxin solid-phase purification column and immunoaffinity column (for complex substrates such as Chinese red pepper, black pepper and chili pepper) 5.5 Reference conditions for mass spectrometry The reference conditions for mass spectrometry are listed below. 5.6 Qualitative determination The retention time of the chromatographic peak of the target compound in the specimen is compared with the retention time of the corresponding standard chromatographic peak, the variation range shall be within ±2.5%. The mass spectrometric ions of each compound must appear, including at least one parent ion and two daughter ions. Meanwhile for the same batch under testing and for the same compound, the allowable deviation between the relative abundance ratio of the two daughter ions of the target compound in the sample and that of the standard solution of equivalent concentration shall not exceed the range as specified in Table 3. 5.7 Production of standard curve Under the analytical conditions of liquid chromatography-tandem mass spectrometry of 5.4 and 5.5, MAKE the standard series solution subject to injection testing in the order from low to high concentration; USE the area ratio of the AFT B1, AFT B2, AFT G1 and AFT G2 chromatogram peaks to each corresponding internal standard chromatogram peak as well as the concentration to make drawing, to obtain the standard curve regression equation, the linear correlation coefficient of which is greater than 0.99. 5.8 Determination of sample solution TAKE the sample solution to be tested which is processed in 5.3; USE the internal standard method to calculate the mass concentration of the target substance in the tested solution. Follow the provisions of clause 6 to calculate the content of the tested substance in the sample. The response value in the 5.9 Blank test DO not weigh the specimen; PERFORM the blank test in accordance with the steps of 5.2 and 5.3.It shall be confirmed that it does not contain substances that interfere with the component to be tested.6 Expression of analytical resultsThe residual amount of AFT B1, AFT B2, AFT G1 and AFT G2 in the specimen is calculated in accordance with formula (1).7 PrecisionThe absolute difference between two independent determinations obtained under repeatability conditions shall not exceed 20% of the arithmetic mean.8 OthersWhen 5 g of the sample is weighed, the detection limit of AFT B1 is 0.03 μg/kg, the detection limit of AFT B2 is 0.03 μg/kg, the detection limit of AFT G1 is 0.03 μg/kg, the detection limit of AFT G2 is 0.03 μg/kg; the limit of quantification of AFT B1 is 0.1 μg/kg, the limit of quantification of AFT B2 is 0.1 μg/kg, the limit of quantification of AFT G1 is 0.1 μg/kg, the limit of quantification of AFT G2 is 0.1 μg/kg.9 PrincipleThe aflatoxin B1, aflatoxin B2, aflatoxin G1, aflatoxin G2 in the specimen are extracted by a mixed solution of acetonitrile-water solution or methanol-water solution, the extract is purified by aflatoxin solid-phase purification column to remove the interfering substances such as fats, proteins, pigments and carbohydrates. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. Tips & Frequently Asked Questions:Question 1: How long will the true-PDF of English version of GB 5009.22-2016 be delivered?Answer: The full copy PDF of English version of GB 5009.22-2016 can be downloaded in 9 seconds, and it will also be emailed to you in 9 seconds (double mechanisms to ensure the delivery reliably), with PDF-invoice.Question 2: Can I share the purchased PDF of GB 5009.22-2016_English with my colleagues?Answer: Yes. The purchased PDF of GB 5009.22-2016_English will be deemed to be sold to your employer/organization who actually paid 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. www.ChineseStandard.us -- GB 5009.22-2016 -- Click this link and select your country/currency to pay, the exact amount in your currency will be printed on the invoice. Full PDF will also be downloaded/emailed in 9 seconds.Question 5: Should I purchase the latest version GB 5009.22-2016?Answer: Yes. Unless special scenarios such as technical constraints or academic study, you should always prioritize to purchase the latest version GB 5009.22-2016 even if the enforcement date is in future. Complying with the latest version means that, by default, it also complies with all the earlier versions, technically.How to buy and download a true PDF of English version of GB 5009.22-2016?A step-by-step guide to download PDF of GB 5009.22-2016_EnglishStep 1: Visit website https://www.ChineseStandard.net (Pay in USD), or https://www.ChineseStandard.us (Pay in any currencies such as Euro, KRW, JPY, AUD).Step 2: Search keyword "GB 5009.22-2016". Step 3: Click "Add to Cart". If multiple PDFs are required, repeat steps 2 and 3 to add up to 12 PDFs to cart. Step 4: Select payment option (Via payment agents Stripe or PayPal). Step 5: Customize Tax Invoice -- Fill up your email etc. Step 6: Click "Checkout". Step 7: Make payment by credit card, PayPal, Google Pay etc. After the payment is completed and in 9 seconds, you will receive 2 emails attached with the purchased PDFs and PDF-invoice, respectively. Step 8: Optional -- Go to download PDF. Step 9: Optional -- Click Open/Download PDF to download PDFs and invoice. See screenshots for above steps: Steps 1~3 Steps 4~6 Step 7 Step 8 Step 9 |
