GB 5009.223-2014 English PDF

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GB 5009.223-2014: National Food Safety Standard -- Determination of ethyl amino acid ethyl ester in food
Status: Valid

Standard ID	USD	BUY PDF	Lead-Days	Standard Title (Description)	Status
GB 5009.223-2014	189	Add to Cart	3 days	National Food Safety Standard -- Determination of ethyl amino acid ethyl ester in food	Valid

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Basic data

Standard ID: GB 5009.223-2014 (GB5009.223-2014)
Description (Translated English): National Food Safety Standard -- Determination of ethyl amino acid ethyl ester in food
Sector / Industry: National Standard
Classification of Chinese Standard: C53
Classification of International Standard: 67.020
Word Count Estimation: 8,833
Date of Issue: 1/28/2015
Date of Implementation: 7/28/2015
Regulation (derived from): National Health and Family Planning Committee Announcement 2015 No. 2
Issuing agency(ies): National Health and Family Planning Commission of the People's Republic of China
Summary: This Standard specifies the beer, wine, wine, liquor and other alcohol and ethyl carbamate in soy sauce by Gas Chromatography - Mass Spectrometry. This Standard applies to the determination of alcohol and beer, wine, wine, liquor and other soy sauce ureth

GB 5009.223-2014: National Food Safety Standard -- Determination of ethyl amino acid ethyl ester in food

---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.
(Determination of the national food safety standards for food in urethane) National Standards of People's Republic of China National Food Safety Standard Determination of ethyl carbamate Published 2015-01-28 2015-07-28 implementation People's Republic of China National Health and Family Planning Commission issued National Food Safety Standard Determination of ethyl carbamate

1 Scope

This standard specifies the beer, wine, rice wine, soy sauce, white wine and other alcoholic and ethyl carbamate content by gas chromatography - mass spectrometry Determination. This standard applies to the determination of soy sauce and a urethane content of beer, wine, rice wine, wine and other alcoholic beverages. Principle 2 After the sample was added D5- urethane internal standard, solid-phase through celite alkaline extraction cartridge eluate was concentrated by gas chromatography Spectrum - mass spectrometer measurement, the amount of internal standard.

3 Reagents and materials

NOTE. Unless otherwise indicated, the reagents used were of analytical grade standard, water as three water GB/T 6682 provisions. 3.1 Reagent 3.1.1 anhydrous sodium sulfate (Na2SO4). 3.1.2 Sodium chloride (NaCl). 3.1.3 hexane (C6H14). chromatography. 3.1.4 ethyl acetate (C4H8O2). chromatography. 3.1.5 ether (C4H10O). chromatography. 3.1.6 methanol (CH4O). chromatography. 3.1.7 basic Celite SPE. packing 4000mg, column capacity 12mL. 3.2 Reagent preparation 3.2.1 anhydrous sodium sulphate. 450 ℃ baking 4h, cooled and then stored in a desiccator. 3.2.2 5% ethyl acetate - ether solution. Take 5mL of ethyl acetate, diluted with ether to 100mL, and mix until use. 3.3 Standard 3.3.1 urethane standards (C3H7O2N, CAS. 51-79-6). purity greater than 99.0%. 3.3.2 D5- urethane standards (C3H2D5NO2, CAS. 73962-07-9). purity greater than 98.0%. 3.4 Standard Preparation 3.4.1 D5- urethane stock solution (1.00mg/mL). 0.01g accurately weighed (accurate to 0.0001g) D5- urethane standard Standard products, dissolved in methanol, the volume to less 10mL, 4 ℃ stored. 3.4.2 D5- using a liquid urethane (2.00μg/mL). Accurately suck D5-urethane stock solution (1.00mg/mL) 0.10mL, With methanol to 50mL, at 4 ℃ or less. 3.4.3 urethane stock solution (1.00mg/mL). 0.05 g of accurately weighed (accurate to 0.0001g) urethane standards, Dissolved in methanol, the volume to 50mL, 4 ℃ below Save to 3 months. 3.4.4 urethane intermediate liquid (10.0μg/mL). Accurately suck urethane stock solution (1.00mg/mL) 1.00mL, with Methanol to 100mL, 4 ℃ below Save to 1 month. 3.4.5 urethane intermediate solution (0.50μg/mL). Accurately suck liquid urethane intermediate (10.0μg/mL) 5.00mL, with A Alcohol volume to 100mL, now with the current. 3.4.6 standard curve working solutions. imbibe liquid urethane intermediate (0.50μg/mL) 20.0μL, 50.0μL, 100.0μL, 200.0μL, 400.0μL and urethane intermediate standard solution (10.0μg/mL) 40.0μL, 100.0μL 1mL volumetric flask to 7 , Each plus 2.00μg/mLD5- urethane used was 100 L, with methanol to volume, to give 10.0ng/mL, 25.0ng/mL, 50.0ng/mL, 100ng/mL, 200ng/mL, 400ng/mL, 1000ng/mL working solution of the standard curve, now Service is used.

4 instruments and equipment

4.1 Gas chromatography - mass spectrometer with electron impact source (EI) source. 4.2 vortex shaker. 4.3 Nitrogen blowing instrument. 4.4 SPE with a vacuum pump. 4.5 ultrasonic cleaning machine. 4.6 muffle furnace. 4.7 Balance. a sense of 0.1mg and 1mg.

5 Step analysis

5.1 Sample Preparation Shake the sample, 2g weighed (accurate to 0.001 g of) the sample (after weighing degassed beer ultrasonic 5min), plus 100.0μL2.00μg/mL After D5- urethane working solution, 0.3 g of sodium chloride (if the sauce is not sodium chloride), sonicate to dissolve, mix, loaded onto celite alkaline solid Phase extraction column under vacuum, the sample solution was slowly penetrate into the extraction column, and allowed to stand 10min. After rinsing 10mL hexane, Solution in diethyl ether/min flow rate to about 1mL eluted, eluant containing 2g anhydrous sodium glass - with 10mL5% ethyl acetate After dehydration funnel, collected in a 10mL graduated test tube, gently blowing with nitrogen at room temperature and about 0.5 mL, diluted with methanol to 1.00mL made It was measured for GC/MS analysis. 5.2 Instrument reference conditions Gas chromatography - mass spectrometer reference conditions. --- capillary column. DB-INNOWAX, 30m × 0.25mm (internal diameter) × 0.25μm (film thickness) column or equivalent; --- Inlet temperature. 220 ℃; --- Column temperature. initial temperature 50 ℃, 1min, to then 8 ℃/min was raised to 180 ℃, the program finishes running, running 240 ℃ for 5min; --- Carrier gas. Helium, purity ≥99.999%, flow rate 1mL/min; --- Ionization mode. Electron ionization (EI), energy of 70 eV; --- quadrupole temperature. 150 ℃; --- Ion source temperature. 230 ℃; --- Transfer line temperature. 250 ℃; --- Solvent delay. 11min; --- Injection mode. splitless; --- injection volume. 1μL ~ 2μL; --- Detection method. selected ion monitoring (the SIM); --- urethane selected ion monitoring (m/z). 44,62,74,89, 62 quantitative ion; --- D5-urethane selected ion monitoring (m/z) 64,76, 64 quantitative ions. 5.3 qualitative determination The method according to measurement conditions and sample standard working solution, a low concentration in the sample qualitatively constant volume can be reduced, the quality of the sample peak retention Time retention time standard substance tolerance of less than ± 2.5%; qualitative ion concentration and the relative abundance of fairly standard working solution Relative abundance does not exceed the allowable deviation in Table 1. The maximum allowable deviation relative ion abundance in Table 1 Qualitative confirmation The relative ion abundance /% > 50 > 20 ~ 50 > 10 ~ 20 ≤10 The maximum permissible deviation /% ± 20 ± 25 ± 30 ± 50 5.4 Quantitative determination of 5.4.1 standard curve prepared The urethane standard curve working solutions 10.0ng/mL, 25.0ng/mL, 50.0ng/mL, 100ng/mL, 200ng/mL, 400ng/mL, 1000ng/mL (containing 200ng/mLD5- urethane) by gas chromatography - mass spectrometer, In the abscissa the concentration of ethyl carbamate, standard curve working solution urethane peak area of the internal standard urethane D5- Peak area ratio of the vertical axis, the standard curve. 5.4.2 Determination of sample The sample solution was measured with a standard curve of the working solution, the sample is calculated in accordance with the content of ethyl carbamate solution assay amino Ethyl content, wherein when a sample containing a low concentration of urethane, should adopt 10.0ng/mL, 25.0ng/mL, 50.0ng/mL, 100ng/mL, 200ng/standard curve working solutions of the standard curve mL; sample containing a high concentration of urethane, the appropriate use of 50.0ng/mL, 100ng/mL, 200ng/mL, 400ng/mL, 1000ng/standard curve working solutions mL of the standard curve. Standard solution mass spectrum given in Appendix A.

6 expression analysis results

Urethane content of the sample according to formula (1). X = c × V × 1000 m × 1000 (1) Where. --- sample X-urethane content, in micrograms per kilogram (μg/kg); C --- Determination of the urethane solution, expressed in nanograms per milliliter (ng/mL); --- constant volume V of liquid sample measured in milliliters (mL); --- m sample weight in grams (G); 1000 --- conversion factor. Results The results of two independent determinations obtained arithmetic mean value under the same condition, three significand reserved.

7 precision

Independent determination of relative deviation of the results obtained in two under repeatability conditions, when the content ≤50μg/kg, not exceeding the arithmetic average 15% of the value; when the content > 50μg/kg, not exceed 10% of the arithmetic mean.

8 Other

When the sample is taken 2g, the method detection limit of urethane 2.0μg/kg, the limit of quantitation was 5.0μg/kg.

Appendix A

Standard solution mass spectrum A.1 urethane and urethane D5- total ion shown in Figure A.1. Figure A.1 urethane and urethane total ion D5- FIG. A.2 urethane spectrum shown in Figure A.2. Figure A.2 urethane spectrum A.3 D5- urethane mass spectrum is shown in Figure A.3. FIG A.3 D5- urethane spectrum 322􀏕 9005 ......

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