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GB 5009.306-2025: National food safety standard - Determination of diphenyl ether 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
Similar standardsGB 5009.306-2025: National food safety standard - Determination of diphenyl ether 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/GB5009.306-2025GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA National Food Safety Standard - Determination of Diphenyl Ether in Foods Issued on: MARCH 16, 2025 Implemented on: SEPTEMBER 16, 2025 Issued by. National Technical Commission of the People’s Republic of China; State Administration for Market Regulation. Table of Contents1 Scope... 3 2 Principle... 3 3 Reagents and Materials... 3 4 Instruments and Equipment... 4 5 Analysis Procedures... 4 6 Expression of Analysis Results... 6 7 Precision... 7 8 Others... 7 9 Principle... 8 10 Reagents and Materials... 8 11 Instruments and Equipment... 8 12 Analysis Procedures... 9 13 Expression of Analysis Results... 11 14 Precision... 11 15 Others... 11 Appendix A Gas Chromatogram of Diphenyl Ether Standard Solution... 12 Appendix B Selected Ion Flow Chromatogram and Ion Mass Spectrum of Diphenyl Ether Standard Solution... 13 National Food Safety Standard - Determination of Diphenyl Ether in Foods1 ScopeThis Standard specifies the determination method of diphenyl ether in foods by gas chromatography and gas chromatography-mass spectrometry. This Standard is applicable to the determination of diphenyl ether in fruits, fruit products, fruit and vegetable juices, and soft candies. Method-I Gas Chromatography2 PrincipleDiphenyl ether in the specimen is extracted with n-hexane; leached by salting out; and the extract liquor is purified by N-propylethylenediamine (PSA) solid phase adsorbent and graphitized carbon black (GCB) solid phase adsorbent; detected by gas chromatograph equipped with hydrogen flame ionization detector; and quantified by external standard method.3 Reagents and MaterialsUnless otherwise specified, all the reagents used in this method are analytically pure; and water is Grade-1 water specified in GB/T 6682. 3.1 Reagents 3.1.1 n-hexane (C6H14). Chromatographically pure. 3.1.2 Sodium chloride (NaCl). 3.1.3 Anhydrous magnesium sulfate (MgSO4). 3.1.4 Sodium citrate (C6H5Na3O7). 3.1.5 Disodium hydrogen citrate (C6H6Na2O7). 3.2 Standard sample Diphenyl ether (Phenyl ether, C12H10O, CAS No.. 101-84-8). Standard substance purity ≥ 99%; or standard sample certified by the state and awarded with a standard substance certificate. 3.3 Preparation of standard solutions 3.3.1 Diphenyl ether standard stock solution (1,000 mg/L). Accurately weigh 10 mg (accurate to 0.1 mg) of diphenyl ether standard sample; dissolve it in n-hexane and make constant volume to 10 mL; store at 4 ℃ in the dark; the validity period is 3 months; or directly purchase a standard solution that meets the traceability requirements. 3.3.2 Diphenyl ether standard intermediate solution (10.0 mg/L). Accurately pipette 0.25 mL of diphenyl ether standard stock solution into a 25 mL volumetric flask; and make constant volume with n-hexane. Store at 4 ℃ away from light; with a validity period of 1 week. 3.3.3 Standard working solution. Accurately pipette 0.50 mL, 1.00 mL, 2.00 mL, 5.00 mL and 10.00 mL of diphenyl ether standard intermediate solution; make constant volume to 10 mL with n-hexane; and prepare standard working solutions with mass concentrations of 0.5 μg/mL, 1.0 μg/mL, 2.0 μg/mL, 5.0 μg/mL and 10.0 μg/mL, respectively. Prepare immediately before use. 3.4 Materials 3.4.1 N-propylethylenediamine (PSA) solid phase adsorbent. Particle size 40 μm~60 μm. 3.4.2 Graphitized carbon black (GCB) solid phase adsorbent. Particle size 120 μm~400 μm.4 Instruments and Equipment4.1 Gas chromatograph. Equipped with hydrogen flame ionization detector (FID). 4.2 Analytical balance. Sensitivity is 0.001 g and 0.000 1 g, respectively. 4.3 Centrifuge. speed ≥ 5,000 r/min. 4.4 Vortex mixer.5 Analysis Procedures5.1 Preparation of specimen Fruit samples refer to GB 2763 Appendix A Food Categories and Test Parts for sampling. Fruit products take the edible part, and soft candy takes the whole; and fully mash them with a masher. Fruit and vegetable juice samples are directly sampled after being fully mixed. The sampling volume shall be no less than 500 g. The prepared specimens shall be placed in a clean container; sealed; labeled with sample information; and tested as soon as possible. 5.2 Extraction 5.2.1 Fruits and fruit and vegetable juices. Weigh 5 g of the specimen (accurate to 0.001 g) in a 50 mL centrifuge tube; add 10 mL of n-hexane; and vortex and oscillate for 1 min. 5.2.2 Fruit products, soft candy. Weigh 5 g of the specimen (accurate to 0.001 g) into a 50 mL centrifuge tube; add 10 mL of warm water at about 50°C; dissolve by ultrasonic for 30 min; accurately add 10 mL of n-hexane; and vortex for 1 min. 5.3 Salting out Respectively weigh 1 g of sodium chloride, 4 g of anhydrous magnesium sulfate, 1 g of sodium citrate, and 0.5 g of disodium hydrogen citrate in a n-hexane-water mixed solution; vortex and mix for 1 min; stand and cool to room temperature. Centrifuge at 5,000 r/min for 5 min; and wait for purification. NOTE. Commercial salt packs with the same adsorbent can also be used directly. 5.4 Purification Transfer 5 mL of the upper-layer n-hexane extract to a centrifuge tube containing 885 mg of anhydrous magnesium sulfate, 150 mg of N-propylethylenediamine (PSA) solid phase adsorbent, and 15 mg of graphitized carbon black (GCB) solid phase adsorbent; vortex and mix for 1 min; centrifuge at 5,000 r/min for 5 min; and take about 1 mL of the upper-layer clear liquid for determination. NOTE. Commercial salt packs with the same adsorbent can also be used directly. 5.5 Instrument reference conditions 5.5.1 Gas chromatography reference conditions The gas chromatography reference conditions are as follows. a) Chromatographic column. 5% phenyl-methyl polysiloxane non-polar column [30 m×0.32 mm (inner diameter), 0.25 μm (film thickness)], or equivalent; b) Chromatographic column temperature. Maintain 80 ℃ for 1 min; increase to 150 ℃ at a heating rate of 10 ℃/min, maintain for 10 min; increase to 280 ℃ at a heating rate of 30 ℃/min, maintain for 1 min; c) Inlet temperature. 285 ℃; d) Carrier gas flow rate. 1.0 mL/min; e) Combustion gas. hydrogen, flow rate of about 30 mL/min; f) Combustion-supporting gas. air, flow rate of about 300 mL/min; Method-II Gas Chromatography-Mass Spectrometry9 PrincipleDiphenyl ether in the specimen is extracted with n-hexane; leached by salting out; and the extract is purified by N-propylethylenediamine (PSA) solid phase adsorbent and graphitized carbon black (GCB) solid phase adsorbent; detected by gas chromatography-mass spectrometry; and quantified by external standard method.10 Reagents and MaterialsUnless otherwise specified, all the reagents used in this method are analytically pure; and water is Grade-1 water specified in GB/T 6682. 10.1 Reagents The same as 3.1. 10.2 Standard sample The same as 3.2. 10.3 Preparation of standard solutions 10.3.1 The same as 3.3.1. 10.3.2 The same as 3.3.2. 10.3.3 Standard working solution. Accurately pipette 0.025 mL, 0.050 mL, 0.100 mL, 0.200 mL and 0.500 mL of diphenyl ether standard intermediate solution; make constant volume to 10 mL with n-hexane; and prepare standard working solutions with mass concentrations of 0.025 μg/mL, 0.050 μg/mL, 0.100 μg/mL, 0.200 μg/mL and 0.500 μg/mL, respectively. Prepare immediately before use. 10.4 Materials The same as 3.4.11 Instruments and Equipment11.1 Gas chromatograph-mass spectrometer. Equipped with electron impact source (EI). 11.2 Analytical balance. The sensitivity is 0.001 g and 0.000 1 g, respectively. 11.3 Centrifuge. speed ≥5,000 r/min. 11.4 Vortex mixer. 11.5 Pipettor. 5 mL, 1 mL, 200 μL.12 Analysis Procedures12.1 Preparation of specimen The same as 5.1. 12.2 Extraction The same as 5.2. 12.3 Salting out The same as 5.3. 12.4 Purification The same as 5.4. 12.5 Instrument reference conditions 12.5.1 Gas chromatography-mass spectrometry reference conditions The gas chromatography-mass spectrometry reference conditions are as follows. a) Chromatographic column. 5% diphenyl-methyl polysiloxane non-polar column [30 m×0.25 mm (inner diameter) 0.25 μm (film thickness)], or equivalent; b) Chromatographic column temperature. Maintain 80 ℃ for 1 min; increase to 150 ℃ at a heating rate of 10 ℃/min, maintain for 10 min; increase to 280 ℃ at a heating rate of 30 ℃/min, maintain for 1 min; c) Inlet temperature. 285 ℃; d) Chromatography-mass spectrometry interface temperature. 280 ℃; e) Ion source temperature. 250 ℃; f) Carrier gas. Helium, Purity ≥ 99.999%, flow rate 1.0 mL/min; g) Injection volume. 1 μL; h) Injection method. Splitless injection, valve opening after 1.0 min; ......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 5009.306-2025 be delivered?Answer: The full copy PDF of English version of GB 5009.306-2025 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 5009.306-2025_English with my colleagues?Answer: Yes. The purchased PDF of GB 5009.306-2025_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. 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