GB 5009.251-2016 PDF EnglishUS$125.00 · In stock · Download in 9 seconds
GB 5009.251-2016: National food safety standard - Determination of 1,2-propylene glycol in food 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 5009.251-2016: National food safety standard - Determination of 1,2-propylene glycol in food---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/GB5009.251-2016GB NATIONAL STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA National Food Safety Standard - Determination of 1,2- propylene glycol in food Issued on. AUGUST 30, 2016 Implemented on. MARCH 01, 2017 Issued by. National Health and Family Planning Commission of PRC Table of ContentsForeword... 4 1 Scope... 5 Method One -- Gas chromatography... 5 2 Principle... 5 3 Reagents and materials... 5 4 Apparatus... 6 5 Analysis steps... 6 6 Expression of analysis results... 9 7 Precision... 9 8 Other... 9 Method Two -- Gas chromatography-mass spectrometry... 9 9 Principle... 10 10 Reagents and materials... 10 11 Apparatus... 11 12 Analysis steps... 11 13 Expression of analysis results... 13 14 Precision... 13 15 Other... 13 Annex A Gas chromatogram of 1,2-propylene glycol standard sample solution ... 14 Annex B Selective ion chromatogram and ion mass spectrum of 1,2-propylene glycol... 15ForewordThis Standard replaces GB/T 23813-2009 “Determination of 1,2-propanediol in foods”, NY/T 1662-2008 “Determination of 1,2-propylene glycol in milk and dairy products - Gas chromatography method”. Compared with GB/T 23813-2009, the main deviations in this Standard are as follows. - modified the standard name as “National Food Safety Standard - Determination of 1, 2-propylene glycol in food”; - added the pretreatment method for milk tablets; - modified the pretreatment methods for milk powder, butter, cream, liquid milk; - added the limit of quantitation of the method. National Food Safety Standard - Determination of 1,2- propylene glycol in food1 ScopeThis Standard specifies the methods that use gas chromatography and gas chromatography-mass spectrometry to determine 1,2-propylene glycol in food. Method One of this Standard is applicable to the determination of 1,2-propylene glycol in pastries, puffed food, cream, cheese, soy products, milk tablets, wet noodle products, frozen drinks, liquid milk, vegetable protein drinks, milk powder, butter, cream. Method Two is applicable to the determination of 1,2- propylene glycol in pastries, puffed food, cheese, soy products, milk tablets, wet noodle products. Method One -- Gas chromatography2 Principle1,2-propylene glycol in the specimen is extracted by absolute ethanol. After the extract is filtered, use gas chromatography to determine. Characterize by retention time. Quantify by external standard method.3 Reagents and materialsUnless otherwise stated, the reagents used in this method are analytically pure, the water is grade two water specified in GB/T 6682. 3.1 Reagents 3.1.1 Anhydrous ethanol (C2H5OH). 3.2 Preparation of reagent 3.2.1 N-hexane saturated acetonitrile solution. Take the same volume of acetonitrile and n-hexane. Place in a separatory funnel. Oscillate. Perform static layering. Take the lower layer solution. 3.2.2 Acetonitrile saturated n-hexane solution. Take the same volume of acetonitrile and n-hexane. Place in a separatory funnel. Oscillate. Perform static layering. Take the upper layer solution. 3.4 Preparation of standard solution 3.4.1 1,2-propylene glycol standard stock solution (10.0 mg/mL). Accurately weigh 1 g of 1,2-propylene glycol standard sample (to the nearest of 0.0001g). Use absolute ethanol to dissolve and transfer to a 100mL volumetric flask. Set volume to the scale. The mass concentration of 1,2-propylene glycol of this solution is 10.0 mg/mL. Store in a refrigerator at 4°C. It shall be valid for 3 months.4 Apparatus4.1 Gas chromatograph (GC). equipped with hydrogen flame ionization detector (FID). 4.4 Vortex mixer. 4.5 Cyclotron oscillator. 4.6 Centrifuge. rotating speed≥8000 r/min.5 Analysis steps5.1 Preparation of specimen 5.1.1 Pastries, puffed food, cheese, soy products, milk tablets The specimen is crushed by the mincer. Accurately weigh 5 g of well-mixed specimen (to the nearest of 0.01g) to a 100mL stoppered conical flask. Add into 50.0 mL of absolute ethanol. Vortex and mix for 2min, then perform oscillation extraction for 40min. After standing for 1h, use 0.45μm organic phase filter membrane to filter. The filtrate obtained is put into gas chromatograph for analysis. 5.1.3 Frozen drinks A solid specimen is placed in a dry beaker to unfreeze. After melting, use a glass rod to smash and stir evenly. The liquid specimen is put at room temperature and shaken evenly. 5.1.4 Liquid milk, vegetable protein drinks Accurately weigh 10 g of well-mixed specimen (to the nearest of 0.01g) into a 50mL stoppered colorimetric tube. Use absolute ethanol to set volume. Vortex and mix for 2min. After standing for 1h (centrifuge at 8000 r/min for 5min if necessary), use 0.45μm organic phase filter membrane to filter. The filtrate obtained is put into gas chromatograph for analysis. 5.1.5 Milk powder Accurately weigh 2 g of well-mixed specimen (to the nearest of 0.01g) into a 50mL stoppered colorimetric tube. Use 8 mL of 40°C water to dissolve and well mix. Use absolute ethanol to set volume. Vortex and mix for 2min. After standing for 1h (centrifuge at 8000 r/min for 5min if necessary), use 0.45μm organic phase filter membrane to filter. The filtrate obtained is put into gas chromatograph for analysis. 5.1.6 Butter, cream Accurately weigh 2 g of well-mixed specimen (to the nearest of 0.01g) into a 50mL stoppered colorimetric tube. Use 6 mL of hexane to dissolve and well mix. Add into 20 mL of n-hexane saturated acetonitrile solution. 5.2 Instrument reference conditions 5.2.1 Chromatographic column. bonded/crosslinked polyethylene glycol stationary phase quartz capillary column, 60m × 0.25mm, 0.25μm, or equivalent column. 5.2.2 Carrier gas. high purity nitrogen; constant current mode, column flow rate of 1.0 mL/min. 5.2.3 Use program temperature rise. Column initial temperature is 80°C. Maintain 1min. Rise temperature to 160°C at 20°C/min. Maintain 2min. Then rise temperature to 220°C at 15°C/min. Maintain 10min. 5.2.9 Injection method. split injection, split ratio of 10.1. 5.3 Production of standard curve Inject the standard series working solutions into the gas chromatograph. Determine the peak area of corresponding 1,2-propylene glycol. The standard curve is drawn by taking the mass concentration of the standard working solution as the abscissa and the peak area of the chromatographic peak as the ordinate.6 Expression of analysis resultsThe content of 1,2-propylene glycol in specimen is calculated according to formula (1).7 PrecisionThe absolute difference between two independent determinations obtained under repeatability conditions shall not exceed 10% of the arithmetic mean.8 OtherWhen the sampling amount is 5 g, the detection limit of this Standard is 0.01 g/kg; the limit of quantification is 0.03 g/kg.9 Principle1,2-propylene glycol in the specimen is extracted by absolute ethanol. After the extract is filtered, use gas chromatography-mass spectrometry to determine. Use selective ion monitoring scan mode (SIM)10 Reagents and materialsUnless otherwise stated, the reagents used in this method are analytically pure, the water is grade two water specified in GB/T 6682. 10.1 Reagents 10.1.1 Anhydrous ethanol (C2H5OH). 10.1.2 Sea sand. 10.1.3 Anhydrous sodium sulfate (Na2SO4). burning 4h at 650°C; store in a sealed dryer, for use. 10.2 1,2-propylene glycol standard product (CH2OHCHOHCH3) Purity≥99.9%. 10.3 Preparation of standard solution11 Apparatus11.1 Gas chromatography-mass spectrometry (GC-MS). EI source. 11.2 Analytical balances. resolutions of 0.01g and 0.0001g. 11.3 Mincer. 11.5 Cyclotron oscillator. ......Source: Above contents are excerpted from the full-copy PDF -- translated/reviewed by: www.ChineseStandard.net / Wayne Zheng et al. 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