Main efficacy and function of pharmaceutical grade sucralose

 Main efficacy and function of pharmaceutical grade sucralose Sucralose SanlüzhetangSucralose C12H19Cl3O8 397.
64 [56038-13-2] This product is 1,6-dichloro-1,6-dideoxy-β-D-fructofuranose-4-chloro -4-Deoxy-α-D-galactofuranoside
.

Calculated according to the dry product, the content of C12H19Cl3O8 should be 98.
0% to 102.
0%
.

【Properties】 This product is white or off-white crystalline powder
.

This product is easily soluble in water, soluble in absolute ethanol, slightly soluble in ethyl acetate
.

Take 1.
0g of this product for specific rotation, accurately weigh it, put it in a 100ml measuring bottle, add water to dissolve and dilute to the mark, shake well, and measure according to the law (General Rule 0621).
The specific rotation is +84.
0° to +87.
5°
.

[Identification] (1) Take 0.
1g of this product, dissolve it in methanol and dilute it to make a solution containing 10mg per 1ml, as the test solution; take another appropriate amount of sucralose reference substance, dissolve it in methanol and dilute it to make each 1ml contains 10mg of solution as a reference solution
.

According to the chromatographic condition test under the related substance inspection item, the position and color of the main spot of the test solution should be the same as the main spot of the reference solution
.

　　(2) In the chromatogram recorded under the content determination item, the retention time of the main peak of the test solution should be consistent with the retention time of the main peak of the reference solution
.

　　(3) The infrared absorption spectrum of this product should be consistent with that of the reference substance (General Rule 0402)
.

　　One of the above (1) and (2) is optional
.

　　[Check] Take 2.
5g of this product from the hydrolyzate, put it in a 10ml measuring bottle, add methanol to dissolve and dilute to the mark, shake well, and use it as the test solution; take an appropriate amount of mannitol reference substance, dissolve it in water and quantitatively dilute it to make each 1ml The solution containing 0.
1g is used as the reference solution (1); another appropriate amount of mannitol and fructose reference substances are taken, dissolved in water and quantitatively diluted to make a mixed solution containing 0.
1g and 0.
4mg per 1ml, as the reference solution (2 )
.

Draw 5 μl of the reference solution (1), (2) and the test solution respectively, and spot them on the same silica gel G thin-layer plate.
The same, after the sampling is completed, spray with a color developer (take 1.
23 g of p-anisidine and 1.
66 g of phthalic acid, add 100 ml of methanol to dissolve, store the solution in a dark place and refrigerate, if the solution fades, it will be invalid) After spraying, at 100 Heated at ℃±2℃ for 15 minutes and inspected immediately against a dark background
.

The spots of the test solution should not be deeper than the spots of the reference solution (2); the reference solution (1) should show white spots, if the spots turn black, that is, the heating time of the TLC is too long, and a retry is required
.

　　Take an appropriate amount of this product for related substances, accurately weigh it, add methanol to dissolve and quantitatively dilute to make a solution containing 0.
1g per 1ml, as the test solution; accurately measure 1ml of the test solution, put it in a 200ml measuring bottle, and use Dilute to volume with methanol as a control solution
.

According to the thin-layer chromatography (general rule 0502) test, draw 5 μl of the test solution and the control solution, respectively, and point them on the same octadecylsilane-bonded silica gel thin layer plate (Whatman Partisil LKC18F plate or thin layer with equivalent performance).
Plate), use 5% sodium chloride solution-acetonitrile (70:30) as developing agent, spread distance 15cm, take out, dry, spray with 15% sulfuric acid methanol solution, heat at 125 ℃ for 10 minutes, and inspect immediately
.

If the test solution shows impurity spots, its color shall not be darker (0.
5%) compared with the main spots of the control solution
.

　　Take about 0.
4g of this product in methanol, accurately weigh it, put it in a headspace bottle, accurately add 2ml of water to dissolve, accurately add an internal standard solution (take an appropriate amount of isopropanol, accurately weigh it, and dilute with water to make a solution containing 0.
1mg per 1ml ) 2ml, sealed and shaken well, as the test solution; another appropriate amount of methanol was taken, accurately weighed, diluted with water to make a solution containing 0.
2mg per 1ml, 2ml was accurately measured, placed in a headspace bottle, and the internal standard was added accurately Solution 2ml, sealed, shaken, as the reference solution
.

Determined according to gas chromatography (general rule 0521), using 6% cyanopropylphenyl-94% dimethylpolysiloxane as the stationary phase; the initial temperature is 35 ° C, maintained for 5 minutes, at a rate of 50 ° C per minute The temperature was raised to 200°C and maintained for 5 minutes; the inlet temperature was 220°C; the detector temperature was 250°C; the equilibration temperature of the headspace vial was 80°C, and the equilibration time was 30 minutes
.

Take the reference solution and the test solution for headspace injection respectively, record the chromatogram, calculate the peak area according to the internal standard method, and the methanol content should not exceed 0.
1%
.

　　Take 0.
5g of this product for moisture and measure it according to the moisture determination method (the first method of General Rule 0832), and the moisture content should not exceed 2.
0%
.

　　Take 1.
0g of this product for the residue on ignition, check it according to the law (General Rule 0841), and the residual residue should not exceed 0.
7%
.

　　Heavy metals and residues left under residue on ignition shall be inspected in accordance with the law (the second method of General Rule 0821), and the heavy metals shall not exceed 10 parts per million
.

　　【Determination of content】 Determined according to high performance liquid chromatography (general rule 0512)
.

　　Chromatographic conditions and system suitability test Octadecylsilane-bonded silica gel was used as filler, water-acetonitrile (85:15) was used as mobile phase, refractive index detector was used, and the flow rate was 1.
0ml per minute
.

The number of theoretical plates shall not be less than 2000 calculated according to the sucralose peak
.

　　Determination method Take an appropriate amount of this product, accurately weigh it, add mobile phase to dissolve and quantitatively dilute to make a solution containing 10mg per 1ml, as the test solution, accurately measure 20μl and inject it into the liquid chromatograph, and record the chromatogram; Sucralose reference substance, determined by the same method
.

According to the external standard method to calculate the peak area, namely
.

　　【Category】Pharmaceutical excipients, flavoring agents and sweeteners,
etc.

　　[Storage] shading, sealed and stored, the temperature does not exceed 25 ℃
.