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Subject content and scope of application
Industry Standard of the People's Republic of China
Food Additive
Isomaltulose
QB1581-92
This standard specifies the product classification, technical requirements, test methods, inspection rules, marking, packaging, transportation and storage of food additive isomaltulose.
This standard applies to isomaltulose made from high-quality white sugar solution through α-glucosyltransferase conversion, concentration, crystallization and separation, which is used as a sweetener in the food industry. 2
Cited Standards
GB8450
Product Classification
Microbiological Examination of Food Hygiene
Determination of Total Colony Count
Microbiological Examination of Food Hygiene
Microbiological Examination of Food Hygiene
Determination of Water Content in Food
Determination of Ash Content in Food
Determination of Copper in Food
Determination of Coliform Group
Test for Salmonella
Determination of Lead in Food Additives
Determination of Arsenic in Food Additives
Chemical Name: 6-O-α—D-pyranoglucopyranosyl-D-fructofuranosyl; Molecular Formula: C12H22011·H20;
Relative Molecular Mass: 342.3 (according to the International Table of Relative Atomic Masses of 1987). 4 Technical requirements
Sensory requirements
White crystals, sweet taste, no peculiar smell, uniform crystals, no lumps, no impurities. Physical and chemical, hygiene indicators
The physical and chemical indicators of isomaltulose shall meet the requirements of Table 1. 4.2.1
Isomaltulose (including crystal water)
Other sugars
The hygiene indicators of isomaltulose shall meet the requirements of Table 2. Table 2
Total number of bacteria, pieces/g
Escherichia coli, pieces/100g
Salmonella
Arsenic (as As)
Lead (as Pb)
Copper (as Cu)
≤350
≤0.00005
—≤0.0001
1≤0.0002
Not detectable
5 Test method
Unless otherwise specified, the reagents and water used in this standard are of analytical grade and distilled water or water of corresponding purity. 5.1 Identification: Thin layer chromatography
5.1.1 Summary of the method
Put the sample on the silica gel G thin layer plate, develop it, and after color development, make a qualitative analysis based on the comparison of the migration value of the sugar on the thin layer plate with the migration value of the standard sample.
5.1.2 Reagents and materials
a. Silica gel G powder;
b. Diphenylamine (GB681);
c. Aniline (GB691);
d. Acetone (GB686);
e. 85% phosphoric acid (GB1282);
f. Boric acid (GB628);
g. Isomaltulose standard solution, 0.005 g/m l Accurately weigh 0.500g analytical pure isomaltulose, dissolve it with a small amount of 80% ethanol solution, transfer it into a 100ml volumetric flask, and dilute it to the scale with 80% ethanol solution; h. Developing agent: chloroform: methanol: acetone: acetic acid = 2:3:2:1; i. Color developer: 1g diphenylamine, add 1ml aniline to dissolve, then add 50ml acetone, mix well, add 5ml 85% phosphoric acid, and store it in a sealed brown reagent bottle (no precipitation should appear). 5.1.3 Instruments and equipment
a. Hair dryer;
b. Chromatography cylinder;
c. Thin layer plate
Preparation of thin layer plate: weigh 6g silica gel G powder, add 15ml of about 0.1mol/L boric acid solution, grind in a mortar for 3-5min, and immediately pour into a coater to make three thin layer plates of 3.5cm×20cm or 5.5cm×20cm, 0.3mm thickness. After drying at room temperature, activate at 110℃ for 1h, take out, and store in a desiccator for later use; d. Microinjector 10μl, 100ul;
e. Sprayer;
f. Coater, dryer, grinder, etc.
5.1.4、Analysis steps
5.1.4.1 Preparation of samples
Weigh 0.500g of isomaltulose powder accurately, dissolve it with a small amount of 80% ethanol solution, transfer it into a 100ml volumetric flask, dilute it to the mark with 80% ethanol solution, and shake it well. 5.1.4.2 Identification method
Spotting: On the baseline 2cm away from the lower end of the thin layer plate, use a microinjector to spot 1ul and 2u1 of the sample, and at the same time spot 1ul and 2u1 of isomaltulose standard solution.
Development and color development: Put the thin layer plate after spotting the sample into the development tank pre-stored with the developer, and the wall of the development tank is affixed with filter paper. When the upper edge of the solvent spreads to 15cm, take it out and evaporate it to dry, spray the color developer, the spot is gray or light green, the background thin plate is white, and the upward movement distance of the sample spot and the standard spot is relatively consistent. 5.2 Determination of content
5.2.1 Summary of method
High pressure liquid chromatography, the sample is treated, separated and determined using a u-BONDADAK-NH2 chromatographic column, and compared with the standard series for quantification.
5.2.2 Reagents and materials
a. Acetonitrile (chromatographic grade);
b. Isomaltulose standard solution 0.010g/ml, accurately weigh 1.000g of isomaltulose (chromatographic grade reagent) that has been vacuum dried at 20℃ for more than 30min, and dilute to 100ml with double distilled water. 5.2.3 Instrument High pressure liquid chromatograph.
5.2.4 Chromatographic conditions
Chromatographic column: μ-BONDADAK-NH2 (diameter 0.45mmX25mm); mobile phase: acetonitrile: water = 7:3;
Flow rate: 0.8~1.0ml/min;
Detector: IR or UV.
Note: Explanation on mobile phase conditions: This composition is not the most suitable. It is best to fine-tune the composition according to the type and state of the packed column, so that the ratio of acetonitrile and water varies between 70:30 and 85:15, make a rough adjustment, and then add a small amount of ethanol for fine adjustment.
5.2.5 Analysis steps
Accurately weigh 0.500g of isomaltulose powder, place it in a 25ml beaker, dissolve it with double distilled water, transfer it all into a 50ml volumetric flask, dilute it to the scale with double distilled water, and shake it well. Take 10μl of standard solution and inject it into the high pressure liquid chromatograph to measure the peak area of isomaltulose. At the same time, inject 10uI of sample solution and compare the measured peak area with the peak area of the standard sample for quantitative analysis. The content of each type of sugar can be calculated by the integrator. 5.2.6 Expression of analysis results
The content of isomaltulose is calculated according to formula (1): A1·V1·S2·VX10**-3
Wherein: X1 isomaltulose content in the sample, %: A1-
-isomaltulose content in isomaltulose standard solution, ug/ul;-volume of isomaltulose standard solution for determination, u1;-injection volume of sample solution, ul;
-volume of diluted sample solution, ml;bzxZ.net
peak area of isomaltulose standard solution; S1
S2——peak area of isomaltulose in sample solution; m—sample mass, g.
5.2.7 Allowable difference
The difference between two parallel determination results shall not exceed 0.20%, and the arithmetic mean shall be taken as the determination result. 5.3 Determination of other sugar content
X=100%-(X1+X2+X3)
Wherein: X—other sugar content, %;
X1—isomaltulose content, %;
X2—water content, %;
X3—ash content, %.
5.4 Determination of water content: in accordance with the provisions of the second method of GB5009.3. 5.5 Determination of ash content: in accordance with the provisions of GB5009.4. .(2)
5.6 Determination of arsenic content: in accordance with the provisions of GB8450. 5.7 Determination of lead content: in accordance with the provisions of GB8449, 5.8 Determination of copper content: in accordance with the provisions of GB5009.13. 5.9 Determination of total bacterial count: in accordance with GB4789.2. 5.10 Determination of coliform group: in accordance with GB4789.3. 5.11 Salmonella test: in accordance with GB4789.4. 6 Inspection rules
6.1 The quality supervision department of the manufacturer shall inspect all items of technical requirements in accordance with the provisions of this standard. The manufacturer shall ensure that all products leaving the factory meet the requirements of this standard. Each batch of products leaving the factory shall be accompanied by a quality certificate, which shall include: manufacturer name, product name, production date, batch number, net weight, proof that the product quality meets this standard and the number of this standard. 6.2 The user has the right to inspect and accept the received products in accordance with the provisions of this standard. 6.3 The weight of each batch of products shall not exceed 5t.
6.4 Sampling method: 2% of the number of bags in each batch shall be sampled, and the small batch shall not be less than 3 bags. When sampling, insert the sampler vertically from the center of the upper part of the packaging bag to three-quarters of the depth of the material layer to sample, and each bag shall be sampled for no less than 50g. Mix the sampled products thoroughly. Use the quartering method to reduce it to 100g and immediately put it into two dry, clean bottles with ground stoppers and seal them. Label the bottles with: manufacturer name, product name, batch number, sampling date and name of the sampler. One bottle is for inspection, and the other bottle is placed in a cool place and kept for one month for reference. 6.5 If one indicator in the test results does not meet the requirements of this standard, re-sampling should be carried out from twice the amount of packaging. Even if the test results show that only one indicator does not meet the requirements, the entire batch of products will be judged as unqualified. 6.6 When the supply and demand parties have objections to the product quality, the two parties may negotiate to select an arbitration unit and conduct arbitration according to the inspection methods specified in this standard.
7 Marking, packaging, transportation, storage
7.1 The packaging bag should have firm and clear markings, including: manufacturer name, product name, production license number, trademark, net weight, batch number or production date, this standard number, factory address and "food additive" sample. 7.2 Packed in paper-plastic composite bags. Each net weight is 25kg, with an allowable error of ±0.2kg. If special packaging is required, the supply and demand parties shall negotiate separately.
7.3 During loading, unloading and transportation, it should be protected from sunlight and rain, and it is strictly forbidden to mix with toxic or contaminated items for shipment. 7.4 It should be stored in a cool and dry place to prevent heat, moisture or sunlight exposure. 7.5 The shelf life is one year.
Additional instructions:
This standard was proposed by the Ministry of Light Industry and the Ministry of Health of the People's Republic of China. This standard is under the jurisdiction of the Food Fermentation Industry Science Research Institute of the Ministry of Light Industry and the Food Sanitation Supervision and Inspection Institute of the Ministry of Health. This standard was jointly drafted by Guangzhou Zhujiang Bioengineering Co., Ltd., Guangdong Food Sanitation Supervision and Inspection Institute, and Guangdong Institute of Microbiology.
The main drafters of this standard are: He Mujie, Dai Yingwei, Xiang Ying, and Wu Chuanbin. This standard refers to the Japanese JSD food review standard. Approved by the Ministry of Light Industry of the People's Republic of China on June 31, 1992 and implemented on April 1, 1993
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