GB/T 20882.4-2021 PDF English
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Quality requirements for starch sugar - Part 4: High fructose syrup
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GB/T 20882.4-2021: PDF in English (GBT 20882.4-2021) GB/T 20882.4-2021
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
ICS 67.180.20
CCS X 31
Replace GB/T 20882-2007
Quality requirements for starch sugar –
Part 4: High fructose syrup
ISSUED ON: DECEMBER 31, 2021
IMPLEMENTED ON: JULY 1, 2022
Issued by: State Administration for Market Regulation;
Standardization Administration of PRC.
Table of Contents
Foreword ... 3
Introduction ... 5
1 Scope ... 6
2 Normative references ... 6
3 Terms and definitions ... 6
4 Product categories ... 7
5 Requirements ... 7
6 Test methods ... 7
7 Inspection rules ... 16
8 Labeling, packaging, transportation, and storage ... 18
Appendix A (Normative) Comparison tables of dry matter (solid matter) content and
refractive index of the high fructose syrup ... 20
Quality requirements for starch sugar –
Part 4: High fructose syrup
1 Scope
This document specifies the quality requirements for high fructose syrup, including
terms and definitions, product classification, requirements, test methods, inspection
rules, labeling, packaging, transportation, and storage.
This document is applicable to the production, inspection, and sale of high fructose
syrup.
2 Normative references
The following documents contain the provisions which, through normative reference in
this document, constitute the essential provisions of this document. For the dated
referenced documents, only the versions with the indicated dates are applicable to this
document; for the undated referenced documents, only the latest version (including all
the amendments) is applicable to this document.
GB/T 191 Packaging - Pictorial marking for handling of goods
GB/T 601 Chemical reagent - Preparations of reference titration solutions
GB/T 602 Chemical reagent - Preparations of standard solutions for impurity
GB/T 603 Chemical reagent - Preparations of reagent solutions for use in test
methods
GB/T 6682 Water for analytical laboratory use - Specification and test methods
3 Terms and definitions
The following terms and definitions apply to this document.
3.1 high fructose syrup
fructose syrup
Starch sugar products whose main components are fructose and glucose that are made
The water used in this method shall meet the water specifications in GB/T6682 unless
other requirements are specified, and the reagents used shall be analytical reagents
unless other specifications are specified. The standard titration solution used in the
analysis, the standard solution for the determination of impurities, preparations, and
products, unless otherwise specified, shall be prepared in accordance with the
provisions of GB/T 601, GB/T 602, and GB/T 603.
Note: Liquid products with crystals can be detected after heating and dissolving in an appropriate way.
6.2 Sensory requirements
Take an appropriate amount of sample, observe the state and color of the sample under
natural light, smell the odor, add pure water at room temperature to prepare a solution
with 10% ~ 15% dry matter, and taste it.
6.3 Fructose and glucose content (calculated as dry matter)
6.3.1 Principle
The components entering the chromatographic column at the same time, due to the
different effects of distribution, size exclusion, or ligand exchange between the mobile
phase and the stationary phase, move at different speeds in the chromatographic column.
After flowing past a certain length of the chromatographic column, they are separated
from each other, and enter the detector in a certain order to generate response signals;
the signals are collected by computer software and processed, and then the
chromatogram and the retention value and peak area or peak height of the components
contained in the sample are obtained. According to the retention time, the qualitative
analysis is carried out by the control method; according to the peak area, the content of
each component is calculated quantitatively.
6.3.2 Reagents and solutions
6.3.2.1 Water: Grade I water in GB/T 6682.
6.3.2.2 Glucose standard (CAS No.: 492-62-6, purity ≥ 98%).
6.3.2.3 Fructose standard (CAS No.: 7660-25-5, purity ≥ 98%).
6.3.2.4 Serial standard solutions of glucose and fructose: Use each sugar standard to
prepare 5 series of standard solutions with different concentrations in the range of 0.5
mg/mL~10.0 mg/mL.
6.3.3 Instruments and equipment
6.3.3.1 High-performance liquid chromatography: it shall be equipped with a
differential refraction detector and a column constant temperature system.
6.3.3.2 Mobile phase vacuum filtration degassing device and 0.2 μm or 0.45 μm
microporous membrane.
6.3.3.3 Electronic balance: The sense quantity shall be 0.0001 g.
6.3.3.4 Micro sampling syringe.
6.3.4 Reference chromatographic conditions
6.3.4.1 Chromatographic column: a cation exchange resin column (with a column
length of 300 mm, an inner diameter of 7.8 mm, and a filler particle size of 5 μm or 9
μm), or a chromatographic column with an equivalent analytical effect.
6.3.4.2 Mobile phase: water.
6.3.4.3 Detector temperature: 45 °C.
6.3.4.4 Column temperature: 85 °C.
6.3.4.5 Flow rate: 0.5 mL/min.
6.3.4.6 Injection volume: 10 μL.
6.3.5 Analysis steps
6.3.5.1 Preparation of the sample solution
Weigh 0.5 g of the sample (calculated as dry matter; the content of various sugar
components shall be within the range of the standard solution series, otherwise the
sampling amount can be added or reduced appropriately), and the weight shall be
accurate to 0.0001 g; dissolve it in water, transfer it to a 50 mL volumetric flask, and
dilute it to the mark with water; shake well, filter it with 0.2 μm or 0.45 μm aqueous
microporous membrane, and leave the filtrate for later use.
6.3.5.2 Drawing of the standard curve
After the series of standard solutions of glucose and fructose are injected respectively,
draw the standard curve according to the concentration of the series of standard
solutions versus the peak area. The linear correlation coefficient shall be above 0.9990.
6.3.5.3 Determination of samples
Inject the prepared sample solution. Qualitatively analyze the chromatographic peaks
of various sugar components in the sample according to the retention time of the
standard. According to the peak area of the sample, calculate the percentage content of
various sugar components by the external standard method or the peak area
normalization method; the external standard method is the arbitration method.
6.4 Dry matter (solid matter)
6.4.1 Instruments and equipment
6.4.1.1 Abbe refractometer: The accuracy shall be 0.0001.
6.4.1.2 Glass rod: The end shall be bent and flat.
6.4.2 Instrument calibration
At 20 °C, the refractive index of the refractometer calibrated with pure water is 1.3330,
which is equivalent to zero content of dry matter (solid matter). The instrument shall be
calibrated at least once a day.
6.4.3 Analysis steps
6.4.3.1 Determination method
Put the refractometer in a place with sufficient light, and adjust the temperature of the
refractometer prism to 20 °C; separate the two prisms, add a small amount of sample
(one drop to two drops) to the fixed prism surface with a glass rod (the glass rod shall
not touch the prism surface, and the time for dropping sample shall be less than 2 s),
immediately close the prism and stay for a few minutes, so that the sample reaches the
temperature of the prism. Adjust the knob of the prism until the field of view is divided
into light and dark parts, turn the compensator knob to eliminate the iridescence and
make the dividing line between light and dark clear; continue to adjust the knob to align
the dividing line between light and dark to the cross line, read the refractive index (the
reading shall be accurate to 0.0001) or content value from the scale, re-read it
immediately, and take the average value as the measured value for one time. Clean and
dry the two prisms, and carry out the second measurement with the same sample
according to the above operation; or, according to Appendix A, obtain the content of
dry matter (solid matter) in the sample by using the refractive index to look-up the table,
and use the looking-up table method as the arbitration method.
6.4.3.2 Result presentation
Take the arithmetic mean of two direct readings as the result for reporting.
6.4.4 Precision
The absolute difference between two independent determination results obtained under
repeatability conditions shall not exceed 1% of their arithmetic mean.
6.5 pH
6.5.1 Principle
Insert the glass electrode (indicating electrode) and the calomel electrode (reference
electrode) into the solution to be measured together to form a battery, the electromotive
force of the battery is related to the pH of the solution, measure the electromotive force
of the battery, and then obtain the pH of the solution.
6.5.2 Instruments
6.5.2.1 pH meter: The accuracy shall be ±0.01 and equipped with an electromagnetic
stirrer.
6.5.2.2 Beaker: 250 mL.
6.5.2.3 Electronic balance: The sense quantity shall be 0.1 g.
6.5.3 Analysis steps
6.5.3.1 Determination method
Debug and calibrate the pH meter according to the instrument manual. Weigh 100 g of
the sample and place it in a clean 250 mL beaker, and put a stir bar in it. Then, rinse the
electrode head with water, and dry it gently with filter paper; then, insert the electrode
into the sample to be tested, turn on the electromagnetic stirrer, and adjust the
temperature compensation; measure the pH of the sample solution, and take the reading
after it is stabilized for 1 min, which is the pH of the sample.
6.5.3.2 Result presentation
The result obtained is rounded to one decimal place.
6.5.4 Precision
The absolute difference between two independent determination results obtained under
repeatability conditions shall not exceed 3% of their arithmetic mean.
6.6 Chroma
6.6.1 Principle
When a beam of parallel monochromatic light passes through a colored solution, the
darker the solution, the greater the absorbance.
6.6.2 Instruments
6.6.2.1 Spectrophotometer: The wavelength range shall be 420 nm~720 nm.
6.6.2.2 Cuvettes.
6.6.2.3 Electronic balance: The sensitivity shall be 0.1 g.
6.8.2 Instruments and equipment
6.8.2.1 Porcelain crucible: 50 mL.
6.8.2.2 High-temperature furnace: The control range of the temperature shall be
525 °C±25 °C.
6.8.2.3 Desiccator: The desiccant shall be silica gel.
6.8.2.4 Analytical balance: The accuracy shall be 0.0001 mg.
6.8.3 Analysis steps
6.8.3.1 The crucible shall be boiled and washed with hydrochloric acid first, then rinsed
with tap water, and then rinsed with distilled water. Put the cleaned crucible in a high-
temperature furnace, and burn it at 525 °C±25 °C for 0.5 h; then open the furnace door,
move the crucible to the furnace mouth, and take it out after it cools to below 200 °C;
put it in a desiccator, cool it to room temperature, and weigh it accurately; repeat
burning until its weight becomes constant (the difference between two weighings is not
more than 0.3 mg).
6.8.3.2 Weigh about 2 g of the sample (the weight shall be accurate to 0.0001 g), and
put it into a crucible that has been burned to constant weight; add 1 mL of concentrated
sulfuric acid dropwise, rotate slowly to make them mix well, place the crucible on an
electric furnace and heat it carefully until the mixture is completely carbonized. Then,
put the crucible in a high-temperature furnace, burn it at 525 °C±25 °C, and keep this
temperature until all the carbonized substances disappear (at least 2 h). Take the crucible
out and cool it, add a few drops of concentrated sulfuric acid to moisten the residue, put
the crucible back into the high-temperature furnace, and burn it until the residue is
completely ashed; open the furnace door, move the crucible to the furnace mouth, and
take it out after it cools to below 200 °C; put it in a desiccator, cool it to room
temperature, and accurately weigh it; repeat burning until its weight becomes constant
(the difference between two weighings is not more than 0.3 mg).
6.8.4 Calculation of the result
The content of the sulfated ash in the sample is calculated according to formula (5):
where:
X4 --- The content of the sulfated ash in the sample, in grams per hundred grams
(g/100g);
m7 --- The mass of the crucible and ash, in grams (g);
m5 --- the mass of the crucible, in grams (g);
m6 --- The mass of the crucible and the sample, in grams (g).
The calculation result is rounded to three decimal places.
6.8.5 Precision
The absolute difference between two independent determination results obtained under
repeatability conditions shall not exceed 5% of their arithmetic mean.
6.9 Light transmittance
6.9.1 Instruments and equipment
Spectrophotometer: The measurable wavelength range shall be 420 nm~720 nm.
6.9.2 Analysis steps
6.9.2.1 Determination method
According to the instrument manual, adjust the zero point and light transmittance of the
instrument at a wavelength of 720 nm. Weigh an appropriate amount of sample, and
prepare the high fructose syrup test solution with a dry matter of 30% by boiled and
cooled (the carbon dioxide is removed) water with a pH of 5.0~7.0. Then, inject the
liquid to be tested into a 1 cm cuvette, and use a spectrophotometer to measure the light
transmittance of the sample liquid at a wavelength of 720 nm, using the same batch of
water as a reference.
6.9.2.2 Result presentation
The result obtained is rounded to one decimal place.
6.9.3 Precision
The absolute difference between two independent determination results obtained under
repeatability conditions shall not exceed 2% of their arithmetic mean.
7 Inspection rules
7.1 Batching
The products of uniform quality, which are continuously produced with the same raw
material, same formula, same process, and from the same production line, are grouped
into a batch.
e) When the national supervisory agency implements random inspection according
to the relevant regulations.
7.5 Judgment rules
7.5.1 After the sample are inspected, and all the inspection items meet the requirements,
then the batch of products can be judged to conform to this document.
7.5.2 If one or two of the inspection items do not meet the requirements, twice the
number of samples shall be taken from the same batch of products for re-inspection,
and the results of the re-inspection shall prevail. If there is still one item that does not
meet the requirements, it shall be judged that the batch of products does not conform to
this document. If there are three or more indicators in the inspection results that do not
meet the requirements, it shall be judged that the batch of products does not conform to
this document.
8 Labeling, packaging, transportation, and storage
8.1 Labeling
8.1.1 The product category shall be indicated on the label or instructions.
8.1.2 The pictorial marking for packaging, storage, and transportation shall meet the
requirements of GB/T 191.
8.2 Packaging
8.2.1 Packaging containers (bottles, barrels, bags, etc.) shall be clean and undamaged.
8.2.2 If the high fructose syrup is transported by tank cars, special tank cars shall be
used.
8.3 Transportation
8.3.1 The means of transport shall be clean.
8.3.2 The high fructose syrup shall not be loaded and transported with toxic, harmful,
corrosive, or odorous items, and shall be protected from moisture, pressure, and
exposure to the sun. When loading and unloading, the high fructose syrup shall be
handled with care, and the package shall not be hooked directly.
8.4 Storage
8.4.1 The high fructose syrup shall be stored in a ventilated, dry, and clean warehouse.
Exposure to the sun and rain shall be avoided, and fire is strictly prohibited.
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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