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GB 5009.120-2025 English PDF

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GB 5009.120-2025: National food safety standard - Determination of protein in foods
Status: Valid

GB 5009.120: Evolution and historical versions

Standard IDContents [version]USDSTEP2[PDF] delivered inStandard Title (Description)StatusPDF
GB 5009.120-2025English219 Add to Cart 3 days [Need to translate] National food safety standard - Determination of protein in foods Valid GB 5009.120-2025
GB 5009.120-2016English90 Add to Cart 0--9 seconds. Auto-delivery National food safety standard - Determination of Sodium Propionate and Calcium Propionate in Foods Valid GB 5009.120-2016
GB/T 5009.120-2003English199 Add to Cart 2 days [Need to translate] Determination of sodium propionate and calcium propionate in foods Obsolete GB/T 5009.120-2003

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Basic data

Standard ID GB 5009.120-2025 (GB5009.120-2025)
Description (Translated English) National food safety standard - Determination of protein in foods
Sector / Industry National Standard
Classification of Chinese Standard X09
Word Count Estimation 11,185
Issuing agency(ies) National Health Commission of the People's Republic of China, State Administration for Market Regulation

GB 5009.120-2016: National food safety standard - Determination of Sodium Propionate and Calcium Propionate in Foods


---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 - Determination of sodium propionate and calcium propionate in foods) National Standards of People's Republic of China National Food Safety Standard Determination of sodium propionate, calcium propionate Issued on.2016-08-31 2017-03-01 implementation People's Republic of China National Health and Family Planning Commission released

Foreword

This standard replaces GB/T 5009.120-2003 "sodium propionate in foods, calcium propionate Determination", GB/T 23382-2009 "Food Zhongbing Sodium, calcium propionate by HPLC. " This standard compared with GB/T 5009.120-2003, the main changes are as follows. --- Standard name was changed to "national food safety standards in food sodium propionate, calcium propionate determination"; --- Increased liquid chromatography; --- GC column by a packed column to capillary column chromatographic conditions change accordingly. National Food Safety Standard Determination of sodium propionate, calcium propionate

1 Scope

This standard specifies the soy products, raw wet noodle products, breads, pastries, vinegar, soy sauce sodium propionate, calcium propionate measurement method. This standard applies to beans products, determination of raw wet noodle products, breads, pastries, vinegar, soy sauce sodium propionate, calcium propionate. The first method of liquid chromatography Principle 2 Propionate in the sample is converted to acid by acidification, ultrasonic water extraction or steam distillation, collected after adjusting pH, by high performance liquid Phase chromatography, wherein the external standard acid content. Samples of sodium propionate and calcium propionate to propionic acid count, when necessary, according to the corresponding parameters Calculate the content of sodium propionate and calcium propionate.

3 Reagents and materials

Unless otherwise indicated, the reagents used were of analytical grade water as a water GB/T 6682 regulations. 3.1 Reagents 3.1.1 phosphoric acid (H3PO4). 3.1.2 diammonium phosphate [(NH4) 2HPO4]. 3.1.3 silicone oil. 3.2 reagent preparation 3.2.1 phosphoric acid solution (1mol/L). After 50mL of water was added 53.5mL phosphoric acid, mix, add water to 1000mL. 3.2.2 diammonium phosphate solution (1.5g/L). Weigh diammonium phosphate 1.5g, dissolved in water and dilute to 1000mL. 3.3 Standard 3.3.1 Standard acid (C3H6O2), CAS. 79-09-4, purity ≥97.0%. 3.3.2 propionic acid standard stock solution (10mg/mL). Weigh 250.0mg acid standard in 25mL volumetric flask, add water to the mark, 4 ℃ stored in the refrigerator for a period of six months.

4 instruments and equipment

4.1 High Performance Liquid Chromatography (HPLC) instrument. with a UV detector or diode array detector. 4.2 Balance. a sense of volume and 0.0001g 0.01g. 4.3 ultrasonic bath. 4.4 centrifuge. speed of not less than 4000r/min. 4.5 Organization mashed machines. 4.6 plug plastic centrifuge tube. 50mL. 4.7 Steam distillation apparatus. 500mL. 4.8 blast oven. 4.9 pH meter. Step 5 Analysis 5.1 Sample Preparation Solid tissue samples were crushed after mixing mashed standby (bread samples need to use drying oven, at 37 ℃ drying 2h ~ 3h conduct Air-dried and placed in tissue stamp mill grinding); after the liquid sample shake up. 5.2 Sample Processing 5.2.1 distillation method (for soy products, raw wet noodle products, vinegar, soy sauce and other samples). After homogenisation of the sample, accurately weighed 25g (accurate to 0.01g), placed in 500mL distillation flask, 100mL of water was added, and then water washing the container 50mL, transferred to a distillation flask, add 1mol/L Phosphoric acid 20mL, 2 to 3 drops of silicone oil drops, steam distillation, the 250mL flask in an ice bath as a liquid absorbing means to be Distilled to remove approximately 240mL when placed 30min at room temperature with 1mol/L phosphate solution pH was adjusted to about 3, add water to the mark Degree, shake, the 0.45μm microporous membrane filtration until the liquid chromatography. 5.2.2 Direct extraction method (for bread, pastries). Accurately weigh 5g (accurate to 0.01g) sample to 100mL beaker, add water 20mL, was added 1mol/L 0.5mL phosphate solution, mixing, ultrasound extraction after 10min, with 1mol/L phosphoric acid solution was adjusted to pH 3 So, transfer the sample to a 50mL volumetric flask, add water to volume, shake. The entire sample was transferred to a 50mL plastic centrifuge tube with a stopper In order to not less than 4000r/min centrifugal 10min, supernatant, after 0.45μm filter membrane until liquid chromatography.

6 instrument reference conditions

6.1 Column. C18 column, 4.6mm × 250mm, 5μm column or equivalent. 6.2 Mobile phase. 1.5g/L diammonium phosphate solution, with 1mol/L phosphoric acid solution was adjusted to pH 2.7 to 3.5 (when using the preparation); by 0.45μm microporous membrane filtration. 6.3 flow rate. 1.0mL/min. 6.4 column temperature. 25 ℃. 6.5 Injection volume. 20μL. 6.6 wavelength. 214nm. 6.7 Cleaning Column Reference conditions. end of the experiment, with 10% methanol wash 1h, then 100% methanol wash 1h.

7 Standard curve drawing

7.1 Distillation. Imbibe stock standard solution 0.5mL, 1.0mL, 2.5mL, 5.0mL, 7.5mL, 10.0mL, 12.5mL placed 500mL distillation flask, before the operation with other sample preparation 5.2.1 final concentration of propionic acid standard solution were 0.02mg/mL, 0.04mg/mL, 0.1mg/mL, 0.2mg/mL, 0.3mg/mL, 0.4mg/mL, 0.5mg/mL, through 0.45μm microporous membrane through Filtration, concentration from low to high injection, the concentration of abscissa to peak area for the vertical axis, the standard curve. 7.2 Direct extraction. Imbibe 5.0mL stock standard solution in 50mL volumetric flask, dilute to the mark with water, preparation of a concentration 1.0mg/mL working standard solution. Then Imbibe working standard solution 0.2mL, 0.5mL, 1.0mL, 2.0mL, 3.0mL, 4.0mL, 5.0mL to 10mL volumetric flask, were added 1mol/L phosphoric acid 0.2mL, water volume to 10mL, and mix. Its acid standard solution The final concentration of solution was 0.02mg/mL, 0.05mg/mL, 0.1mg/mL, 0.2mg/mL, 0.3mg/mL, 0.4mg/mL, 0.5mg/mL, through 0.45μm filter membrane, from low to high concentration of the injection, the concentration of abscissa, the peak area of the vertical axis, standard curve line.

8 Determination of the sample solution

The treated sample solution into the machine with a standard series of the same test. Calculated concentration of propionic acid in the sample according to the standard curve. Propionic acid response test sample solution should be within the linear range of the standard curve, beyond the linear range should be diluted before injection analysis.

9 expression analysis

Samples sodium propionate (Ca) content (acid dollars), according to equation (1). X = c × V × 1000 m × 1000 × f (1) Where. X --- sample sodium propionate (Ca) content (acid basis), in units of grams per kilogram (g/kg); c --- from a standard curve obtained sample liquid acid concentration, in milligrams per milliliter (mg/mL); V --- volume of the sample solution final volume in milliliters (mL); m --- sample weight in grams (g); f --- dilution. Sample measured acid content multiplied by the conversion factor of 1.2967, that was the content of sodium propionate; Sample measured acid content multiplied by the conversion factor of 1.2569, that was the content of calcium propionate. The results to three significant figures. 10 Precision Two independent determination results under the absolute difference in repeatability condition must not exceed 10% of the arithmetic mean. Other 11 Sampling of 25g, constant volume when the volume of 250mL, propionic acid detection limit of 0.03g/kg, the limit of quantification of 0.10g/kg. Gas Chromatography Method II Principle 12 Propionate in a sample by acidifying into propionic acid, directly into the GC by steam distillation after collection, with hydrogen flame ionization detector Detected, retention time qualitative, wherein the content of external standard acid. Samples of sodium propionate and calcium propionate to propionic acid count, when needed, can be According to the corresponding parameters were calculated content of sodium propionate and calcium propionate. 13 Reagents and materials Note. Unless otherwise indicated, the reagents used were of analytical grade water as a water GB/T 6682 regulations. 13.1 Reagents 13.1.1 phosphoric acid (H3PO4). 13.1.2 acid (CH2O2). 13.1.3 silicone oil. 13.2 reagent preparation 13.2.1 phosphoric acid solution (1090). Take 10mL phosphoric acid with water to 100mL. 13.2.2 formic acid (298). Take 1mL acid with water to 50mL. 13.3 Standards Propionic acid standard (C3H6O2), CAS. 79-09-4, purity ≥97.0%. 13.4 Standard Solution 13.4.1 acid standard stock solution (10mg/mL). Weigh 250.0mg acid standard in 25mL volumetric flask, add water to the mark Degree, 4 ℃ stored in a refrigerator for a period of six months. 13.4.2 acid standard solution. The stock solution is diluted with water to 10μg/mL ~ 250μg/mL standard series, the Pro with the existing service. 14 instruments and equipment 14.1 Gas chromatograph. with flame ionization detector. 14.2 Balance. the amount of 0.0001g sense and a sense of the amount of 0.01g. 14.3 steam distillation apparatus. 14.4 blast oven. 15 analysis steps 15.1 Sample Preparation With 5.1. 15.2 sample processing After homogenisation of the sample, accurately weighed 25g, (bread samples need to use drying oven, 37 ℃ dried 2h ~ 3h air-dried and placed RESEARCH Mortar grinding), placed in 500mL distillation flask, 100mL of water was added, and then water washing the container 50mL, transferred to a distillation flask, add 10mL solution of phosphoric acid, 2 to 3 drops of silicone oil drops, steam distillation, distillation rate of 2 drops/s ~ 3 drops/s, will be placed in 250mL flask Ice bath as a liquid absorbing means to be near 250mL distillation removed, placed 30min at room temperature, add water to the mark. Mixing, gas phase color Spectral analysis. 15.3 Instrument Reference conditions 15.3.1 Column. polyethylene glycol (PEG) fused silica capillary column, column length 30m, an inner diameter of 0.25mm, the film thickness of 0.5μm or equivalent Column. 15.3.2 Carrier gas. nitrogen, purity > 99.99%. 15.3.3 carrier gas flow rate. 1mL/min. 15.3.4 Inlet temperature. 250 ℃. 15.3.5 Split ratio. 10.1. 15.3.6 detector temperature. 250 ℃. 15.3.7 oven temperature. 125 ℃ to maintain 5min, then 15 ℃/min rate rose to 180 ℃, holding 3min. 15.3.8 Injection volume. 1μL. 15.4 standard curve Take the standard series standards using various concentrations of liquid 10mL, add 0.5mL of formic acid solution and mix. Which are injected into the GC Instrument to measure the corresponding peak areas or high concentration of the standard working solution as abscissa and the response (peak area or peak height) as ordinate plotted Prepared standard curve. 15.5 Determination of the sample solution Draw 10mL sample solution prepared in (15.1) in a test tube, was added 0.5mL of formic acid solution, and mix with the standard series of the same into the machine test. Calculated concentration of propionic acid in the sample according to the standard curve. 16 analysis results presentation Samples sodium propionate (Ca) content (acid dollars), according to equation (2). X = m × (2) Where. X --- sample sodium propionate (Ca) content (acid basis), in units of grams per kilogram (g/kg); c --- from a standard curve obtained sample liquid acid concentration, in micrograms per milliliter (μg/mL); m --- sample weight in grams (g); V --- the final volume of the sample solution, in milliliters (mL); 1000 --- μg/g converted to g/kg coefficients. Sample measured acid content multiplied by the conversion factor of 1.2967, that was the content of sodium propionate; Sample measured acid content multiplied by the conversion factor of 1.2569, that was the content of calcium propionate. The arithmetic mean of two under the same condition of independent determination results indicated that the results to three significant figures. 17 Precision Two independent determination results under the absolute difference in repeatability condition must not exceed 10% of the arithmetic mean. Other 18 Sampling of 25g, constant volume when the volume of 250mL, propionic acid detection limit of 0.03g/kg, the limit of quantification of 0.10g/kg.

Appendix A

Standard Substance chromatogram GC Figure A.1 acid standard substance Standard Substance acid gas chromatogram is shown in Figure A.1. GC Figure A.1 acid standard substance LC Figure A.2 acid standard substance Liquid chromatogram acid standard material is shown in Figure A.2. Figure A.2 liquid chromatogram acid standard substance

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