GB/T 23529-2009Trehalose (English PDF)

6.3 Hygiene requirements

It shall comply with the relevant provisions of the State.

7.1 Sensory test

TAKE an appropriate amount of samples; under the natural light, OBSERVE the color

and shape of the sample visually; inspect whether there are impurities; TAKE a small

amount of samples; TASTE them carefully (before tasting the second sample, it shall

gargle with water); MAKE a record.

7.2 Content (High performance liquid chromatography)

7.2.1 Principle

Each component that comes into the chromatographic column at the same time - due

to the difference of dissolution, adsorption, permeation and ion exchange between

mobile phases and stationary phases - is allocated repeatedly for several times

between two phases of the chromatographic column along with the mobile phases.

Due to the moving speeds of each component in the chromatographic column are

different, after passing through the chromatographic column of a certain length, the

components are separated from each other, flow out the chromatographic column

sequentially, and flow into the signal detector. INDICATE the spectral peak values of

each component on the recorder or on the data processing device. QUANTIFY by

normalization method or external standard method according to retention time.

7.2.2 Instruments

7.2.2.1 High performance liquid chromatograph (equipped with a differential detector).

7.2.2.2 Mobile phase degasser and 0.45µm microporous membrane.

7.2.2.3 Chromatographic column. amino column (4.6mm×300mm, 5µm).

7.2.2.4 Analytical balance. a sensitivity of 0.0001g.

7.2.2.5 Micro injector. 10µL.

7.2.3 Reagents

7.2.3.1 Water. secondary distilled water or ultrapure water.

7.2.3.2 Acetonitrile. chromatographically pure.

7.2.3.3 Trehalose standard products. purity >= 99.5%.

Note. If it takes crystalline trehalose as standard products, then the purity of anhydrous

trehalose shall be multiplied by a conversion factor (342.30 / 378.33 = 0.90).

7.2.4 Analysis steps

7.2.4.1 Standard product preparation

The standard products need to be dried in a 60°C electro-thermal constant-

temperature oven for 5h for weighing. WEIGH about 0.5g of trehalose standard

products (7.2.3.3), accurate to 0.0001g; DISSOLVE with water (7.2.3.1) and dilute to

50mL; SHAKE well. FILTER with 0.45µm microporous membrane (7.2.2.2); COLLECT

the filtrate for determination.

7.2.4.2 Sample preparation

The samples need to be dried in a 60°C electro-thermal constant-temperature oven for

5h for weighing. WEIGH about 0.5g of trehalose samples (7.2.3.3), accurate to

0.0001g; DISSOLVE with water (7.2.3.1) and dilute to 50mL; SHAKE well. FILTER with

0.45µm microporous membrane (7.2.2.2); COLLECT the filtrate for determination.

7.2.4.3 Determination of samples

The mobile phase is acetonitrile . water = 70 . 30. TURN on the differential detector

before the day of determination, PREHEAT till stable, FIT on the column, INLET the

mobile phase with a flow rate of 0.1mL / min, BALANCE overnight. Before formal

injection analysis, INLET the mobile phase used TO the reference cell for more than

20min, RESTORE normal flow path, to make the mobile phase flow through the sample

cell, ADJUST the flow rate to 1.0mL / min, ADJUST the baseline until the baseline is

stable, INLET 10L of the standard solution (7.2.4.1) and the prepared sample (7.2.4.2)

respectively. According to the retention time of standard products, determine the

chemical composition of the sugar components in the sample. According to the peak

area of the sample, calculate the percentage content of sugar components by external

standard method.

7.2.4.4 Calculation results

WEIGH 30g of the sample, accurate to 0.1g; ADD water to dissolve and dilute to

100mL; SHAKE well. USE 1cm cuvette to take water as the blank control;

DETERMINE the absorbance of the sample solution at the wavelength of 420nm and

720nm respectively; RECORD the readings.

7.6.3 Calculation results

7.6.3.1 Chromaticity

CALCULATE the chromaticity according to formula (4).

Where.

X4 - Colorimetric values of samples;

OD420 - Absorbance of sample solution at the wavelength of 420nm;

OD720 - Absorbance of sample solution at the wavelength of 720nm.

7.6.3.2 Turbidity

The turbidity value of samples is the absorbance of samples at the wavelength of

720nm.

7.6.4 Precision

The absolute difference between the two independent determination results obtained

under the repeatability conditions shall not exceed 0.2% of the arithmetic mean.

8.1 The products dried at a time are deemed as one batch. The maximum batch shall

not exceed the output per shift.

8.2 Each batch of products shall exit factory after being inspected as qualified by the

inspection department of...

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