Some standard content:
ICS67.180.20
Classification number: X31
Registration number: 15118-2005
Light Industry Standard of the People's Republic of China
QB/T1216-2004
Replaces QB/T1216-1991
High fructose syrup
High fructose syrup
Published on December 14, 2004
National Development and Reform Commission of the People's Republic of China, June 2005 -01 Implementation
QB/T1216—2004
Normative references
Product classification
Analysis methods
Inspection rules
Marking, packaging, transportation, storage
Appendix A (Normative Appendix) Comparison table of solid content of fructose syrup [% (mass fraction)] and refractive index
QB/T1216-2004
This standard is a revision of QB/T1216-1991 "Fructose syrup and its test methods". This revision mainly refers to the International Society of Beverage Technology (ISBT) standard.
Compared with QB/T1216-1991, the main changes of this standard are as follows: F55 type products are added;
Product classification is deleted;
- "DE value\ and \cyanide\ indicators are deleted; "color" unit is changed to "RBU\, and the indicators are modified accordingly: - "glucose + fructose" and "insoluble particles" indicators are added. Appendix A of this standard is a normative appendix.
This standard is proposed by China Light Industry Federation. This standard is under the jurisdiction of the National Food Fermentation Standardization Center. The drafting units of this standard are: Shandong Baolingbao Biotechnology Co., Ltd., China Food Fermentation Industry Research Institute, Shandong Luzhou Group, Anhui Fengyuan Biochemical Co., Ltd., Dacheng-Cargill High Fructose (Shanghai) Co., Ltd., Shanghai Haocheng Food Development Co., Ltd., Guangdong Xinyi Sugar Co., Ltd.
The main drafters of this standard are: Zhang Anguo, Guo Xinguang, Niu Jichao, Cai Qihai, Liang Zhi, Zhong Hangping, Zhu Lihong. This standard was first issued in 1991, and this is the first revision. This standard replaces the light industry standard QB/T1216-1991 "Fructose-glucose syrup and its test methods" issued by the former Ministry of Light Industry from the date of implementation.
1 Scope
Fructose-glucose syrup
QB/T1216-2004
This standard specifies the product classification, requirements, analysis methods, inspection rules and marking, packaging, transportation and storage of fructose-glucose syrup. This standard applies to sugar solution obtained by enzymatic hydrolysis of starchy raw materials and then converted into fructose-glucose syrup by glucose isomerase. 2 Normative references
The clauses in the following documents become the clauses of this standard through reference in this standard. For all dated referenced documents, all subsequent amendments (excluding errata) or revisions are not applicable to this standard. However, the parties to the agreement based on this standard are encouraged to study whether the latest versions of these documents can be used. For all undated referenced documents, the latest versions shall apply to this standard. GB/T191 Pictorial marking for packaging, storage and transportation
GB/T4789.2 Microbiological examination of food hygiene Determination of total colony countGB/T4789.3 Microbiological examination of food hygiene Determination of coliform group
GB/T4789.4 Microbiological examination of food hygiene Test for Salmonella
GB/T5009.11
Determination of total arsenic in food
GB/T5009.12 Determination of lead in food GB/T5009.34: Determination of sulfite in food GB/T6682 Specifications and test methods for water for analytical laboratories QB/T2319 Liquid glucose
Food Hygiene Law of the People's Republic of China
3 Product classification
According to the fructose content, it is divided into:
- Fructose syrup with a fructose content of not less than 42% (on dry matter). Type 42 (F42) - Type 55 (F55) - fructose syrup with a fructose content of not less than 55% (percentage of dry matter). 4 Requirements 4.1 Sensory requirements The syrup is a colorless or light yellow, transparent, viscous liquid. It has a mild sweetness, a unique aroma of fructose syrup, and no peculiar smell. There are no impurities visible to normal vision. 4.2 Physical and chemical indicators Should comply with the provisions of Table 1. 4.3 Hygiene indicators Should comply with the provisions of Table 2.
QB/T1216—2004
Dry matter (solids) (mass fraction)/%Fructose (in solids) (mass fraction)/%Glucose + fructose (in dry matter) (mass fraction)/%pH
Chroma/RBU
Insoluble particles/(mg/kg)
Sulfated ash/%
Transmittance/%
Table 1 Physical and chemical indicators
The measured value of dry matter shall not exceed ±0.5% (mass fraction) of the indicated value. Table 2 Hygiene indicators
Sulfur dioxide/(mg/kg)
Arsenic/(mg/kg)
Lead/(mg/kg)
Total colony count/[cfu/mL (or g)]
Escherichia coli/[MPN/100g (or mL)
Pathogenic bacteria (Salmonella)
5 Analytical method
Not detectable
Unless otherwise specified, only analytically pure reagents shall be used. Water, GB/T6682, Grade III (including Grade III) or above. F55
5.1 Sensory test
Put about 30mL of sample in a colorless, clean and dry sample cup (or 50mL small beaker), place it in a bright place, observe its color and transparency with naked eyes, check whether there are impurities visible to normal vision, and use a glass rod to take an appropriate amount of sample and put it in the mouth to taste its taste (before tasting the second sample, use clean water to stimulate the mouth). Keep a record. 5.2 Dry matter (solids)
Determine according to QB/T2319, and after measuring the refractive index, check Appendix A "Fructose syrup solid content [% (mass fraction)] and refractive index comparison table" to obtain the dry matter content.
5.3 Fructose and glucose content (HPLC method) 5.3.1 Principle
Each component entering the chromatographic column at the same time is repeatedly distributed between the two phases of the chromatographic column with the mobile phase due to the different dissolution, adsorption, penetration or ion exchange between the mobile phase and the stationary phase. Due to the different movement speeds of each component in the chromatographic column, after passing through a certain length of the chromatographic column, they are separated from each other, flow out of the chromatographic column in sequence, enter the signal detector, and the peak values of each component are displayed on the recorder or data processing device. The qualitative analysis is carried out according to the retention time, and the quantitative analysis is carried out according to the peak area using the external standard method. 5.3.2 Instruments
5.3.2.1 High performance liquid chromatograph (equipped with a differential refractometer and a column thermostat system). 5.3.2.2 Mobile phase vacuum filtration degassing device and 0.2μum or 0.45μm microporous membrane. QB/T1216—2004
5.3.2.3 Chromatographic column: calcium or potassium cation exchange resin column (filler particle size: 5μm: column size: @7.8mm×300mm) or amino bonded column (filler particle size: 5um; column size: @4.6mm×250mm), or chromatographic column with equivalent analytical effect. 5.3.2.4 Analytical balance: sensitivity 0.1mg. 5.3.2.5 Micro-injector: 50uL.
5.3.3 Reagents
5.3.3.1 Water: double distilled water or ultrapure water. 5.3.3.2 Acetonitrile: chromatographic grade (for amino column). 5.3.3.3 The purity of the standard of glucose, fructose, maltose and maltotriose should be above 95%. Use the standard of each sugar to prepare 6 standard solutions with different mass concentrations in the range of 0.5mg/mL to 10mg/mL. 5.3.4 Analysis steps
5.3.4.1 Preparation of sample solution
Weigh 0.5g of sample (in terms of dry matter, the content of various sugar components should be within the range of the standard solution series, otherwise the sampling amount can be appropriately increased or decreased) to an accuracy of 0.0001g, dissolve in water, transfer to a 50mL volumetric flask and make up to volume with water, filter with a 0.2um or 0.45μm aqueous microporous membrane, and set aside the filtrate.
5.3.4.2 Chromatographic conditions
Cation exchange resin column: The mobile phase is pure water. The day before the measurement, turn on the power of the differential refractive index detector, preheat and stabilize it, install the chromatographic column, adjust the column temperature to 85°C, and pass the mobile phase at a flow rate of 0.2mL/min to equilibrate overnight. Before the formal injection analysis, the mobile phase used was input into the reference cell at a flow rate of 0.5mL/min for more than 20 minutes, and then restore the normal flow path to allow the mobile phase to pass through the sample cell, maintaining a flow rate of 0.5mL/min for baseline, and the sample can be injected after the baseline is stable. The injection volume is 10μL~20μL. Amino bonded column: mobile phase is acetonitrile: water = 75:25 (volume ratio). The day before the measurement, turn on the power of the differential refractive index detector, preheat and stabilize, install the chromatographic column, adjust the column temperature to 40℃, and pass the mobile phase at a flow rate of 0.1mL/min to balance overnight. Before the formal injection analysis, the mobile phase used is input into the reference cell at 1.0mL/min for more than 10min, and then restore the normal flow path to allow the mobile phase to pass through the sample cell, maintaining a flow rate of 1.0mL/min for baseline, and the sample can be injected after the baseline is stable. The injection volume is 10μL~20μL. 5.3.4.3 Drawing a standard curve
After injecting a series of standard solutions of glucose, fructose, maltose, and maltotriose, a standard curve is drawn with the mass concentration of the standard sample versus the peak area. The linear correlation coefficient should be above 0.9990. 5.3.4.4 Determination of samples
Inject the prepared sample solution. According to the retention time of the standard, the chromatographic peaks of various sugar components in the sample are qualitatively determined. According to the peak area of the sample, the content (mass fraction) of various sugar components is calculated by the external standard method. 5.3.4.5 Calculation of results
The content of various sugars in the sample is checked by the standard curve or calculated according to formula (1), and the value is expressed in %. 4xm
V×100
Wherein:
Content of a certain sugar in the sample (mass fraction, in dry matter), %;
The peak area of a certain sugar in the sample;
The mass of a certain sugar standard in the standard sample, in grams (g);
The dilution volume of the standard sample, in milliliters (mL): (1)
QB/T1216-2004
The peak area of a certain sugar standard in the standard sample;The mass of the sample (in dry matter), in grams (g);The dilution volume of the sample, in milliliters (mL). The calculation result is rounded to the nearest integer.
5.3.4.6 Allowable difference
The difference between two determination results of the same sample shall not exceed 5% of the average value. 5.4pH
5.4.1 Principle
Insert the glass electrode (indicator electrode) and the calomel electrode (reference electrode) into the solution to be tested to form a battery. The electromotive force of the battery is related to the pH of the solution. The electromotive force of the battery is measured to obtain the pH of the solution. 5.4.2 Instruments
5.4.2.1 pH meter: accuracy is ±0.01, with electromagnetic stirrer. 5.4.2.2 Beaker: 250mL.
5.4.2.3 Balance: sensitivity 0.1g.
5.4.3 Analysis steps
5.4.3.1 Instrument calibration
Debug and calibrate the instrument at 25℃ according to the instrument manual. 5.4.3.2 Measurement
Weigh an appropriate amount of sample and place it in a clean beaker, then put a magnetic rotor in it, then insert the electrode into the sample to be tested, turn on the electromagnetic stirrer, adjust the temperature compensation, measure the pH of the sample solution, and read the value after the pH stabilizes for 1 minute. The result is expressed to one decimal place.
5.5 Chroma
5.5.1 Principle
When a beam of parallel monochromatic light passes through a colored solution, the darker the color of the solution, the greater the absorbance. 5.5.2 Instruments
5.5.2.1 Spectrophotometer: wavelength range 420nm~720nm. 5.5.2.2 Colorimetric meter: 4cm×1cm or 1cm×1cm. 5.5.2.3 Balance; sensitivity 0.1g.
5.5.3 Analysis steps
Put the sample with a substance content of 50% (mass fraction) into a cuvette and use water as a blank to adjust the zero point. Measure its absorbance at 420nm and 720nm wavelengths respectively.
5.5.4 Result calculation
The chromaticity of the sample is calculated according to formula (2).
In the formula:
X=(420 -2×A20)
Lx0.61478
The chromaticity of the sample, in RBU;
The absorbance of the sample at a wavelength of 420nm:
The absorbance of the sample at a wavelength of 720nm;
The value of the thickness of the colorimetric blood, in centimeters (cm);x1000
The number of grams of sugar in each milliliter of syrup [dry matter is 50% (mass fraction)]. (2)
5.6 Insoluble particles
5.6.1 Apparatus
5.6.1.1 Vacuum filtration device: one set.
5.6.1.2 Microporous filter membrane: pore size 0.8μm. 5.6.1.3 Weighing blood.
5.6.1.4 Vacuum drying oven.
5.6.1.5 Dryer: use color-changing silica gel as desiccant. 5.6.2 Analysis steps
QB/T1216-2004
Weigh 500g of sample into a 2L beaker, add 1L of hot water (about 80℃), and stir to dissolve it completely. Place the weighed microporous filter membrane on the funnel, slowly pour the dissolved sample solution into it, vacuum filter, and wash the precipitate with 200mL of hot water (about 80℃). Place the filter membrane in weighing III, vacuum dry at 100℃ for 1h, take it out, cover it, place it in a desiccator to cool for 30min, take out the filter membrane and weigh it. 5.6.3 Calculation of results
The insoluble particulate matter content of the sample is calculated according to formula (3). X= (m,-m)x10
Wherein:
The insoluble particulate matter content of the sample, in milligrams per kilogram (mg/kg): The value of the mass of the filter membrane plus the residue after drying, in grams (g); The value of the mass of the filter membrane, in grams (g): The value of the mass of the weighed sample, in grams (g). 5.7 Sulfate ash
Determine according to QB/T2319.
5.8 Transmittance
5.8.1 Principle
When a beam of parallel monochromatic light passes through a solution, the absorbance of the solution is proportional to the concentration of the solution and the thickness of the liquid layer. The smaller the absorbance of the solution, the greater the transmittance and the clearer and more transparent the solution. 5.8.2 Instruments
5.8.2.1 Spectrophotometer: wavelength range 420nm~720mm. 5.8.2.2 Balance: sensitivity 0.1g.
5.8.3 Analysis steps
5.8.3.1 Sample solution preparation
Take an appropriate amount of sample and dilute it with water to 30% (mass fraction) of dry matter for later use. 5.8.3.2 Determination
Put the sample solution into a 1cm colorimetric III, use water as a blank to adjust the zero point, measure its transmittance at a wavelength of 720nm, which is the transmittance result of the sample, expressed to one decimal place.
5.9 Sulfur dioxide
Determine according to GB/T5009.34.
Determine according to GB/T5009.11.
Determined according to GB/T5009.12.
QB/T1216-2004
5.12 Total colony count
Determined according to GB/T4789.2.
5.13 Coliform bacteria
Determined according to GB/T4789.3.
5.14 Pathogenic bacteria (Salmonella)
Determined according to GB/T4789.4.
6 Inspection rules
6.1 Batch
Products produced with the same raw materials, formula and process are considered a batch with one batch of materials, and the maximum batch should not exceed the shift output. Each batch of products shall be inspected and qualified by the inspection department of the manufacturer before leaving the factory, and shall be accompanied by a product quality certificate. 6.2 Sampling
6.2.1 For bottled and barreled products, samples shall be drawn according to the provisions of Table 3 and Table 4 respectively. Table 3 Sampling table for bottled samples
Batch range/box
100~250
251~500
Batch range/barrel
50~100
6.2.2 For products in tank trucks, each truck must be inspected.
Number of samples to be drawn/box
Table 4 Sampling table for barreled samples
Number of unit packages to be drawn/bottle
Number of samples to be drawn/barrel
6.2.3 For products in barrels and tank trucks, samples shall be drawn from 10 cm below the liquid surface, and the sampler shall comply with food hygiene standards. 6.2.4 The sampling volume of each tank truck product should be no less than 2kg; the sampling volume of each barrel product should be no less than 1kg; the total sampling volume of bottled products should be no less than 2kg.
6.2.5 After mixing the sample, divide it into two parts and seal them. Paste a label and indicate the product name, manufacturer name and address, batch number, sampling date and location, and name of the sampler on the label. One part will be sent to the laboratory for inspection, and the other will be sealed and kept for half a month for future reference. When doing microbiological inspection, the sampler and glass bottle should be sterilized in advance (the sample must not touch the bottle mouth). 6.3 Factory inspection
6.3.1 Before the product leaves the factory, the quality inspection department of the manufacturer shall be responsible for batch inspection according to the provisions of this standard. Only products that meet the requirements of the standard and have signed the quality certificate can leave the factory.
6.3.2 Items of factory inspection: sensory requirements, dry matter, fructose, fructose + glucose, pH, transmittance, insoluble particles, total bacterial count.
6.4 Type inspection
6.4.1 Items of type inspection: In addition to the items specified in 6.3.2, sulfated ash, sulfur dioxide, arsenic, lead, pathogenic bacteria, and coliform bacteria shall also be inspected.
6.4.2 Under normal circumstances, type inspection shall be carried out once a quarter. It shall also be carried out when one of the following situations occurs. 6
Change of main raw and auxiliary materials:
Change of key processes and equipment:
When the new trial-produced product or the normal production product is stopped for more than 3 months and then resumes production: When the national quality supervision agency conducts random inspection. 6.5 Judgment rules
QB/T1216-2004
If 1 to 2 indicators are unqualified in the test results, samples of twice the amount should be taken from the same batch of products for re-testing, and the re-testing results shall prevail. If there is still one unqualified, the batch of products shall be judged as unqualified. 7 Marking, packaging, transportation, purchase and storage
7.1 Marking
7.1.1 The outside of the product packaging container shall be marked with: product name, manufacturer name, net content, batch number, production date, shelf life and adopted standard number.
The packaging storage and transportation diagram shall be implemented in accordance with the provisions of GB/T191. 7.1.2
7.2 Packaging
7.2.1 The packaging container shall be clean, sanitary, and undamaged, and shall comply with the relevant provisions of the "Food Hygiene Law of the People's Republic of China". 7.3 Transportation, Purchase and Storage
7.3.1 During transportation, measures should be taken to prevent dust, flies, exposure to the sun, and chrysanthemum rain. It is strictly forbidden to mix and transport with toxic, harmful, corrosive substances and pollutants. The loading and unloading should comply with the requirements of the packaging storage and transportation diagram. 7.3.2 The finished products should be stored in a cool, dry, ventilated and clean warehouse and shipped out according to the first-in-first-out principle. This product should be stored at 28℃～32℃.
7.3.3 The precipitation of crystals during storage does not affect the product quality. QB/T1216-2004
Solids
Appendix A
(Normative Appendix)Www.bzxZ.net
Comparison table of solid content of fructose syrup [% (mass fraction)] and refractive indexTable A.1
Refractive index
Solids
F42 product
Refractive index
Solids
Refractive index
Solids
Refractive index
Solids
Table A.1 (continued)
Refractive index
1,40733
Solids
QB/T1216
6-2004
Refractive index
1,40572
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