Pharmaceutical grade sucrose stearate 2025 pharmacopoeia filing A

Pharmaceutical grade sucrose stearate 2025 pharmacopoeia filing A

Pharmaceutical grade sucrose stearate 2025 pharmacopoeia filing A

Sucrose stearate

Zhetang Yingzhisuanzhi

Sucrose Stearate

This product is a mixture of stearic acid esters of sucrose, prepared by reacting methyl stearate from plant sources with sucrose. There is a distillation step in the process of fatty acid methylation. According to the relative content of monoesters, diesters, triesters and above, they are divided intoⅠaTheⅠbTheⅡTheⅢThe four models should comply with the provisions in the table below.

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【 Appearance 】 This product is a white to off white powder.

Acid value of this product3gPrecise weighing and positioning250mlAdd isopropanol to a conical flask-Water（2∶1）Mixed liquid[Add phenolphthalein indicator solution before use1.0ml, using * titrant（0.1mol/L）Adjust to a slightly pink color display]50mlDissolve with slight heat and determine according to the law (General rules)0713）The acid value should not exceed6.0.

【 Identification 】（1）Take this product0.5gAdd n-butanol20mland5%sodium chloride solution20mlThe mixture (preheated to)40～60℃）Shake to dissolve, let it stand, separate the water layer, and reuse the n-butanol layer5%sodium chloride solution40ml(Preheat to40～60℃）Divide2Wash again, take about the n-butanol layer2mlPlace it in a test tube, tilt the tube, and slowly add anthrone test solution along the wall3mlTo form a layered structure, place60℃water bath heating3In minutes, blue to green appears at the contact surface between the two liquid layers.

（2）In the chromatogram recorded under the fatty acid composition item, the retention time of the methyl palmitate peak and the methyl stearate peak in the test solution should be consistent with the retention time of the corresponding peak in the reference solution.

【 Inspection 】 Take an appropriate amount of free sucrose, weigh it accurately, and add diluent[*-Water（87.5∶12.5）]Dissolve and quantitatively dilute to make each1mlModerate content50mgThe solution is used as the test sample solution.

Take an appropriate amount of sucrose reference standard, weigh it accurately, dissolve it in diluent separately, and dilute it quantitatively to make each one1mlModerate content0.2mgThe0.5mgThe1.0mgThe2.0mgand2.5mgThe solution is used as a reference solution.

According to the General Principles of High Performance Liquid Chromatography (HPLC)0512）Measurement. Using amino bonded silicone as a filler; with0.001%（g/ml）Acetonitrile solution of ammonium acetate as mobile phaseA, in order to0.001%（g/ml）Ammonium acetate*-Water（90∶10）Solution as mobile phaseBPerform gradient elution according to the table below; Detection using an evaporative light scattering device (reference condition for low-temperature shunt mode: drift tube temperature)45℃The flow rate of the carrier gas is per minute3.0LReference conditions for high-temperature diversion mode: drift tube temperature65℃The flow rate of the carrier gas is per minute2.0LOther modes of detectors can be set according to actual situations.

Take a low concentration reference solution20μlInject into the liquid chromatograph and record the chromatogram. The signal-to-noise ratio of the sucrose peak should be greater than10The separation degree of each adjacent peak should meet the requirements.

Accurately measure the reference solution and the test solution separately20μlInject into the liquid chromatograph separately, record the chromatogram, and calculate the linear regression equation and correlation coefficient based on the logarithm of the concentration of the reference solution and the logarithm of the corresponding peak area（r）Should not be less than0.99Calculate the content of free sucrose in the test sample using a linear regression equation, without exceeding4%.

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Moisture content of this product0.5gAccording to the moisture determination method (general rules)0832The First Law1）Measurement, moisture content should not exceed4%.

Burning residue: Take this product1.0gInspect in accordance with the law (General Principles)0841）The remaining residue shall not be passed over1.5%.

The residue left under the category of ignition residue for heavy metals shall be determined in accordance with the law (General Rules)0821The second method states that the content of heavy metals shall not exceed 20 parts per million.

Fatty acid composition of this product0.1gAccording to the law (General Principles)0713）； Take appropriate amounts of reference standards of methyl laurate, methyl tetradecanoate, methyl palmitate, and methyl stearate, dissolve them in n-hexane and dilute to make each one1mlEach of them contains approximately0.1mgThe solution is used as a reference solution.

According to the area normalization method, the content of lauric acid and tetradecanoic acid should not exceed3%Palmitic acid should be25%～40%Stearic acid should be55%～75%The total amount of palmitic acid and stearic acid shall not be less than90%.

According to the molecular exclusion chromatography method (general rules)0514）Measurement.

Styrene for chromatographic conditions and system suitability testing-Diethylbenzene copolymer as filler（7.8mm×30cm, 5μmTwo chromatography columns connected in series or chromatography columns with equivalent efficiency; Using * as the mobile phase; Differential refractive index detector. The order of peak emergence is multi ester, diester, and monoester with three or more esters, and the separation degree between diester peak and monoester peak shall not be less than1.2The separation degree between the monoester peak and the stearic acid peak should meet the requirements.

Measurement method: Take an appropriate amount of this product, weigh it accurately, dissolve it in mobile phase, and dilute it quantitatively to make each sample1mlModerate content15mgThe solution is filtered and used as the test sample solution for precise measurement20μlInject into the liquid chromatograph, record the chromatogram, and calculate the content of monoester, diester, triester, and above esters according to the following formula.

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In the formulaAFor the determination results of free sucrose,%；

BFor the measurement results under the moisture item,%；

CFor the calculation of free fatty acids,%；

XThe peak area of monoester;

YThe peak area of diester;

ZThe sum of peak areas of triglycerides and above.

[Category] Solvent additives, emulsifiers, lubricants, etc.

【 Storage 】 Seal and store in a dry place.

[Label] The type of this product should be indicated.