This standard specifies the determination method of allura red in food. This standard is applicable to the determination of allura red in candy packaged foods. When the sampling volume of this standard is 10g, the detection limit is 5mg/kg. The linear range is 0mg/L～12mg/L. GB/T 5009.141-2003 Determination of allura red in food GB/T5009.141-2003 Standard download decompression password: www.bzxz.net

1CSB7.040
National Standard of the People's Republic of China
G/T5009.141—2003
Replaces GB/T16346-1996
Determination of allura red in foods
Determination of allura red in foods2003-08-11Promulgated
Ministry of National Construction of the People's Republic of China
Standardization Administration of China
2004-07-01Implementation
GB/I5009.141—2003
This standard replaces GB/716345—1996Determination of allura red in foodsThis standard is compiled according to GB/T16346-1996 Thermal Principles Part 4, Chemical Analysis Methods 3. The structure of the original standard has been modified. ||This standard was proposed and coordinated by the Ministry of Health of the People's Republic of China. The drafting units of this standard are: Food Hygiene Inspection and Quarantine Institute of the Ministry of Health, Hebei Provincial Epidemic Prevention Station, Municipal Health Epidemic Prevention Station. The main drafters of this standard are: Chang Zuying, Li Liangxue, Hong Shuting, Gong Ping, Fei Lihua. The original standard was issued in 199e. This is the first time. The first scope: 210
Determination of allura red in food
This standard does not define the determination method of allura red in food. This standard is applicable to the determination of allura red in candy coating and other foods. GB/T 5009.141—2003
When the sampling volume of this standard is 10, the detection limit is 58. The linear range is 0mg/1.-12mg/. 2 Principle
The red is attached to the hydroxyl group under acidic conditions, adsorbed on the surface in the alkaline solution, and then separated by chromatographic potential, and compared with the standard for qualitative and quantitative analysis.
3 Bin Ya
3.1 Shi 306
3.2 Shen alcohol.
3.3 Polyamide powder (Long Long 6): 200 days
3. Number, i+1u.
3. 5g/I. Argon sodium chloride.
3.6 Sea sand: light salt (1+0 boiled 15min, washed with water to neutral, then boiled with ice machine 15C/1. for 15min, washed with water to neutral, then dried at 105 degrees, stored in a bottle, each press, 3.760% fast fraction) ethyl ester,
3.8 ethyl ester-oxygen liquid; take 2ml of nitrogen water, dilute 79% (volume fraction) ethanol to 100m: 3.92H16 water: use 205% tablets to fill up to 2H6: 3.102008/I. Nitric acid melt. bZxz.net
3. 111093 No. 1. Sodium dodecanoate solution.
3.t2 Standard solution of inductively coupled red: Confirm the amount of inductively coupled red to be 0.01 g/mL, add water to dissolve, and adjust to 25 mL to obtain 1 g/mL.
3.13 Standard solution of inductively coupled red: Add 5 mL of standard inductively coupled red to a 50 mL volume, add water to 50 mL to obtain 0.1 mg/mL
3.14 Developing agent
3.14. t Dicalcium hydroxide + water-hydrogenated water (7+3-3 1-6.5). 3.14.2 Alcohol + anhydrous alcohol + 1 to hydrogenated water (6+2+3) 3.14,32.5 Sodium citric acid-ammonia water + ethanol (8+1+2). 4 Apparatus
4,1 can be used as a photometer.
4.2 Micro-drawing injector, 0l.
4.3 Rotary drawing
4.4 Self-adjusting machine
4.5 Filter paper: medium-speed treading paper, color selection reverse currency
4.6 Constant water bath pot,
4.7 Check and select centrifugal clear.
GB/T50Q9.141—2003
5 Analysis steps
5. Treatment of test samples
5.1.1 Soda: Heat the sample to remove carbon dioxide. Weigh 1.0% of the sample into a beaker and adjust the pH with 20% lemon balm. Add ~1.1% amide to the sample to remove the adsorbed pigment. Transfer all the sample powder to a warm hopper and filter. Wash with H400 aqueous hot water for several times (about 200 μl) to wash out substances such as sugar. If there is natural pigment, wash with methanol-neutralized aldehyde solution for 1-3 times, and wash for 20 minutes until the washing liquid becomes dark red. Then wash with 70% water several times until the extract is neutral. The washing process must be thoroughly exhausted. Then use ethanol and ammonia water to desorb the color in batches. Collect all the desorbed liquid, dry and remove ammonia. Evaporate to about 2mL, transfer to a 5mL volumetric bottle, continue to wash with 3% ethanol in batches, and add 5ml. Put it into a volumetric cabinet and adjust to the scale with 5% ethanol. This drop is used for paper chromatography.
5.1.2 Hard extract: weigh 10.0g of crushed sample: add 30mL of water, heat and dissolve. If the pH value of the sample is high, adjust it to about 4 with citric acid (3.10). The following is in accordance with *5,1.1 "0.5g--1. Add adsorption...".
5.1.3 Pastry: weigh 10.0g of crushed sample, add 30mL of unsaturated fat to extract fat, extract three times in total, blow it down with a hair dryer after boiling, and put it into a funnel. Desorb the pigment with 1% alcohol, evaporate it to 20mL with water, add 1% sodium calcium phosphate to precipitate blue, vacuum evacuate, desorb the red pigment on the paper with ethanol, and then put the solution in a water bath to deoxygenate, adjust the pH to acidic, and the following is in accordance with "5.1.1 Soda \"Add 10.0g of the sample and add 15mL of petroleum aldehyde to remove fat. Take it twice, pour off the residual aldehyde, and then evaporate the petroleum aldehyde in 50% water, then add ethanol-ammonia desorption liquid to desorb the red, and add 10TmL of desorption liquid to evaporate until the desorption is colorless. Drain the desorption water to remove ethanol, and when the volume is about 20m, add 1ml. (1119). 1m of gelatin precipitate and place it for 2min, then add 1ml of ammonia to make the pH alkaline, transfer the solution to a centrifuge tube at 5300l/ml, centrifuge for 15min, pour off the supernatant, remove the ethanol in water, and then use lemon to adjust the pH to 3.10, and follow the steps below. 1. Add 0.5 g to 0.0 g of amine powder to the soda water for adsorption. Start the operation. 5.2 Qualitative analysis Take chromatographic paper and spot 3 μl of 1 μl or sample treatment solution and 1 μl of chromatographic solution on the starting line 2 cm away from the magnet. Hang them in the developing medium containing 3.14.1, 14.2, 3.14.3 developing agents respectively. Develop with the upward method. When the diving front reaches 15 m, take the chromatographic paper out and let it air dry for ten minutes. Compare it with the standard spot for qualitative analysis. 5.3 Quantification
5.3.1 Preparation of standard curve
Pick 0.00.2, .4, 0.6, 0.8, 1.m red-sensitive standards into 10L colorimetric tubes respectively, add water to each tube up to the scale, use an 11ml colorimetric cup and adjust the zero point with a zero tube, measure the absorbance at a wavelength of 500nm, and draw a standard curve: 5.3.2 Determination of sample
Take chromatographic paper: On the starting line 2cm away from the bottom, apply 0.20mL of liquid to the test rod, and make a strip from left to right. The standard sample of the system is 1 point of the sensitive red, according to the method of unfolding, press the air out, cut the sample ribbon, apply it several times with a small amount of hot water, and transfer it to 1mL of colorimetric solution. Add water and dilute until it is dark. After mixing, measure the source light intensity at 50Cnm with the standard at the same time. Calculation of results
The content of sensitive red in the sample is calculated according to the following formula: A X1 000
Where:
X—the content of sensitive red in the sample, in grams (kg/k))212
--the content of sensitive red in the sample solution, in grams (kg)
V\--the total volume after equalization, in liters (a). -. The volume of the sample layer, in liters (m). The results are retained to two significant figures.
7 Precision
FB/T5G9.1A1-2003
The absolute difference between the results of the nanometer measurement obtained under the condition of stability shall not exceed 19% of the technical mean. 2E3
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