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Main functions and effects of pharmaceutical grade glyceryl behenate Shanyusuan GanyouzhiGlyceryl Dibehenate This product is a mixture of mono-, di- and triglycerides, mainly containing glyceryl behenate
.
By behenic acid and glycerol obtained by esterification
.
The content of monoglycerides should be 15.
0% to 23.
0%, diglycerides should be 40.
0% to 60.
0%, and triglycerides should be 21.
0% to 35.
0%
.
【Properties】This product is white or off-white powder or hard wax block; it has a slight odor
.
This product is soluble in , almost insoluble in water or ethanol
.
Melting point The melting point of this product (general rule 0612) is 65～77℃
.
Acid value The acid value of this product (general rule 0713) should not be greater than 4.
0
.
Iodine value Take 3.
0g of this product and measure it according to the law (general rule 0713).
The iodine value should not be greater than 3.
0
.
Peroxidation value The peroxide value of this product (general rule 0713) should not be greater than 6
.
Saponification value The saponification value (general rule 0713) of this product should be 145～165
.
[Identification] (1) In the chromatogram recorded under the content determination item, the retention time of the three main peaks of the test solution should be consistent with the retention time of the corresponding three main peaks of the reference solution
.
(2) In the chromatogram recorded under the fatty acid composition, the retention time of the main peak of the test solution should be consistent with the retention time of the methyl behenate peak in the reference solution
.
[Check] Take the test solution under the content determination item for free glycerol as the test solution; take another 0.
1g glycerol reference substance, accurately weigh it, put it in a 25ml measuring bottle, dissolve it with tetrahydrofuran and dilute it to the mark, shake well, Precisely measure 0.
25ml, 0.
5ml, 1.
0ml and 2.
5ml, put them in weighed 25ml measuring bottles respectively, add 5.
0ml of tetrahydrofuran to each measuring bottle, shake well, weigh, and calculate the amount of solution in each measuring bottle per 1g.
The number of milligrams of glycerol, as a standard curve solution of different concentrations
.
According to the chromatographic conditions under the content determination item, accurately measure 40 μl of the standard curve solution, inject them into the liquid chromatograph respectively, record the chromatogram, and calculate the linear regression equation with the peak area and the corresponding concentration, and the correlation coefficient (r) should not be less than 0.
995
.
Precisely measure 40 μl of the test solution, inject it into a liquid chromatograph, record the chromatogram, and calculate the glycerol content in the test solution by a linear regression equation, and the free glycerol should not exceed 1.
0%
.
Moisture Take an appropriate amount of this product, use pyridine as a solvent, and measure it according to the moisture determination method (General Rule 0832 First Method 1), and the moisture content should not exceed 1.
0%
.
Residue on ignition Take 1.
0g of this product and inspect it according to the law (General Rule 0841), and the residual residue should not exceed 0.
1%
.
Preparation of nickel reference solution: Precisely measure 1ml of nickel single element standard solution (1.
000g/L), put it in a 200ml measuring bottle, dilute it with water to the mark, shake well, accurately measure 5ml, put it in a 100ml measuring bottle, and dilute with water to Scale, shake well, accurately measure 0.
5ml, 1.
0ml, 1.
5ml and 2.
0ml, put them in 25ml measuring bottles respectively, add 0.
5ml of 1% magnesium nitrate solution, 0.
5ml of 10% ammonium dihydrogen phosphate solution and 6ml of nitric acid respectively, Dilute with water to the mark, shake well, and that’s it
.
Preparation of the test solution: Take 0.
25g of this product, accurately weigh it, put it in a polytetrafluoroethylene digestion tank, add 6ml of nitric acid and 2ml of concentrated hydrogen peroxide solution (30%), mix well, cover the inner cover, and screw it tightly Put the jacket into a suitable microwave digestion furnace for digestion.
After the end, take out the digestion tank, let it cool, add 2 ml of concentrated hydrogen peroxide solution (30%), and repeat the above digestion steps
.
After the digestion is complete, remove the inner tank and place it on an electric hot plate to slowly heat until the reddish-brown steam evaporates, let it cool, quantitatively transfer the contents to a 25ml volumetric flask with water, add 1% magnesium nitrate solution and 10% ammonium dihydrogen phosphate Each solution is 0.
5ml, diluted with water to the mark, shaken up, and ready; the reagent blank solution is prepared in the same way
.
Determination method Take the reagent blank solution, the test solution and the reference solution, use the graphite furnace as the atomizer, and measure it at the wavelength of 232.
0 nm according to the atomic absorption spectrophotometry (general rule 0406 first method), calculate, and get
.
The nickel content shall not exceed 0.
0001%
.
Heavy metals Take the residues left under the item of residue on ignition, and inspect them according to the law (the second method of general rule 0821), and the heavy metals shall not exceed 10 parts per million
.
Arsenic salt take 1.
0g of this product, add 1.
0g of calcium hydroxide, mix, add water and stir evenly, after drying, first burn with small fire to carbonize, then burn at 500～600℃ to completely ashed, let cool, add 5ml of hydrochloric acid and 23ml of water should be checked according to the law (the first method of General Principle 0822) and should meet the regulations (0.
0002%)
.
The fatty acid composition takes 0.
1g of this product and is determined according to the law (General Rule 0713); respectively take methyl palmitate, methyl stearate, methyl arachidic acid, methyl behenate, methyl erucate, methyl behenate An appropriate amount of ester reference substance, adding n-heptane to make a solution containing about 0.
1mg per 1ml, as a reference substance solution
.
According to the area normalization method, the content of palmitic acid should not exceed 3.
0%, stearic acid should not exceed 5.
0%, arachidic acid should not exceed 10.
0%, behenic acid should not exceed 83.
0%, and erucic acid should not exceed 3.
0%.
Alkanoic acid should not exceed 3.
0%
.
【Determination of content】According to size exclusion chromatography (general rule 0514)
.
Chromatographic conditions and system suitability test: Styrene-divinylbenzene copolymer is used as filler (7.
8mm×30cm, 5μm, two chromatographic columns are connected in series or chromatographic columns with equivalent performance); Tetrahydrofuran is used as mobile phase; Differential refractive index detection The temperature of the column is 35°C, the temperature of the detector is 35°C, and the temperature of the injector is 35°C (the temperature of the test solution should be kept at 35°C to avoid precipitation of the sample)
.
The peaks of triglyceride, diglyceride, monoglyceride and glycerol appear in sequence (refer to the attached chromatogram), the separation degree of diglyceride peak and monoglyceride peak should meet the requirements, and the diglyceride peak and triglyceride peak should meet the requirements.
The degree of separation shall not be less than 1.
0
.
Determination method Take 0.
2g of this product, accurately weigh it, put it in a weighed 25ml volumetric flask, add 5.
0ml of tetrahydrofuran, slightly heat it in a 35°C water bath, shake to dissolve, take it out, and weigh it as the test solution , accurately measure 40 μl and inject it into the liquid chromatograph, and record the chromatogram; another appropriate amount of the reference substance of glyceryl behenate is taken, accurately weighed, dissolved in tetrahydrofuran and quantitatively diluted to make a solution containing about 40 mg per 1 ml, and the same method is used for determination.
.
Calculate the content of free glycerol, monoglyceride, diglyceride and triglyceride in the test solution according to the following formula
.
In the formula, A is the measurement result under the item of free glycerol, %; B is the measurement result under the moisture item, %; D is the calculation result of free fatty acid; 340.
58 is the molecular weight of behenic acid; 56.
11 is the molecular weight of potassium hydroxide; X is the test solution The sum of the peak areas of monoglycerides and free fatty acids; Y is the peak area of diglycerides in the test solution; Z is the peak area of triglycerides in the test solution
.
【Category】Pharmaceutical excipients, lubricants and release blockers,
etc.
【Storage】Keep tightly closed
.
.
By behenic acid and glycerol obtained by esterification
.
The content of monoglycerides should be 15.
0% to 23.
0%, diglycerides should be 40.
0% to 60.
0%, and triglycerides should be 21.
0% to 35.
0%
.
【Properties】This product is white or off-white powder or hard wax block; it has a slight odor
.
This product is soluble in , almost insoluble in water or ethanol
.
Melting point The melting point of this product (general rule 0612) is 65～77℃
.
Acid value The acid value of this product (general rule 0713) should not be greater than 4.
0
.
Iodine value Take 3.
0g of this product and measure it according to the law (general rule 0713).
The iodine value should not be greater than 3.
0
.
Peroxidation value The peroxide value of this product (general rule 0713) should not be greater than 6
.
Saponification value The saponification value (general rule 0713) of this product should be 145～165
.
[Identification] (1) In the chromatogram recorded under the content determination item, the retention time of the three main peaks of the test solution should be consistent with the retention time of the corresponding three main peaks of the reference solution
.
(2) In the chromatogram recorded under the fatty acid composition, the retention time of the main peak of the test solution should be consistent with the retention time of the methyl behenate peak in the reference solution
.
[Check] Take the test solution under the content determination item for free glycerol as the test solution; take another 0.
1g glycerol reference substance, accurately weigh it, put it in a 25ml measuring bottle, dissolve it with tetrahydrofuran and dilute it to the mark, shake well, Precisely measure 0.
25ml, 0.
5ml, 1.
0ml and 2.
5ml, put them in weighed 25ml measuring bottles respectively, add 5.
0ml of tetrahydrofuran to each measuring bottle, shake well, weigh, and calculate the amount of solution in each measuring bottle per 1g.
The number of milligrams of glycerol, as a standard curve solution of different concentrations
.
According to the chromatographic conditions under the content determination item, accurately measure 40 μl of the standard curve solution, inject them into the liquid chromatograph respectively, record the chromatogram, and calculate the linear regression equation with the peak area and the corresponding concentration, and the correlation coefficient (r) should not be less than 0.
995
.
Precisely measure 40 μl of the test solution, inject it into a liquid chromatograph, record the chromatogram, and calculate the glycerol content in the test solution by a linear regression equation, and the free glycerol should not exceed 1.
0%
.
Moisture Take an appropriate amount of this product, use pyridine as a solvent, and measure it according to the moisture determination method (General Rule 0832 First Method 1), and the moisture content should not exceed 1.
0%
.
Residue on ignition Take 1.
0g of this product and inspect it according to the law (General Rule 0841), and the residual residue should not exceed 0.
1%
.
Preparation of nickel reference solution: Precisely measure 1ml of nickel single element standard solution (1.
000g/L), put it in a 200ml measuring bottle, dilute it with water to the mark, shake well, accurately measure 5ml, put it in a 100ml measuring bottle, and dilute with water to Scale, shake well, accurately measure 0.
5ml, 1.
0ml, 1.
5ml and 2.
0ml, put them in 25ml measuring bottles respectively, add 0.
5ml of 1% magnesium nitrate solution, 0.
5ml of 10% ammonium dihydrogen phosphate solution and 6ml of nitric acid respectively, Dilute with water to the mark, shake well, and that’s it
.
Preparation of the test solution: Take 0.
25g of this product, accurately weigh it, put it in a polytetrafluoroethylene digestion tank, add 6ml of nitric acid and 2ml of concentrated hydrogen peroxide solution (30%), mix well, cover the inner cover, and screw it tightly Put the jacket into a suitable microwave digestion furnace for digestion.
After the end, take out the digestion tank, let it cool, add 2 ml of concentrated hydrogen peroxide solution (30%), and repeat the above digestion steps
.
After the digestion is complete, remove the inner tank and place it on an electric hot plate to slowly heat until the reddish-brown steam evaporates, let it cool, quantitatively transfer the contents to a 25ml volumetric flask with water, add 1% magnesium nitrate solution and 10% ammonium dihydrogen phosphate Each solution is 0.
5ml, diluted with water to the mark, shaken up, and ready; the reagent blank solution is prepared in the same way
.
Determination method Take the reagent blank solution, the test solution and the reference solution, use the graphite furnace as the atomizer, and measure it at the wavelength of 232.
0 nm according to the atomic absorption spectrophotometry (general rule 0406 first method), calculate, and get
.
The nickel content shall not exceed 0.
0001%
.
Heavy metals Take the residues left under the item of residue on ignition, and inspect them according to the law (the second method of general rule 0821), and the heavy metals shall not exceed 10 parts per million
.
Arsenic salt take 1.
0g of this product, add 1.
0g of calcium hydroxide, mix, add water and stir evenly, after drying, first burn with small fire to carbonize, then burn at 500～600℃ to completely ashed, let cool, add 5ml of hydrochloric acid and 23ml of water should be checked according to the law (the first method of General Principle 0822) and should meet the regulations (0.
0002%)
.
The fatty acid composition takes 0.
1g of this product and is determined according to the law (General Rule 0713); respectively take methyl palmitate, methyl stearate, methyl arachidic acid, methyl behenate, methyl erucate, methyl behenate An appropriate amount of ester reference substance, adding n-heptane to make a solution containing about 0.
1mg per 1ml, as a reference substance solution
.
According to the area normalization method, the content of palmitic acid should not exceed 3.
0%, stearic acid should not exceed 5.
0%, arachidic acid should not exceed 10.
0%, behenic acid should not exceed 83.
0%, and erucic acid should not exceed 3.
0%.
Alkanoic acid should not exceed 3.
0%
.
【Determination of content】According to size exclusion chromatography (general rule 0514)
.
Chromatographic conditions and system suitability test: Styrene-divinylbenzene copolymer is used as filler (7.
8mm×30cm, 5μm, two chromatographic columns are connected in series or chromatographic columns with equivalent performance); Tetrahydrofuran is used as mobile phase; Differential refractive index detection The temperature of the column is 35°C, the temperature of the detector is 35°C, and the temperature of the injector is 35°C (the temperature of the test solution should be kept at 35°C to avoid precipitation of the sample)
.
The peaks of triglyceride, diglyceride, monoglyceride and glycerol appear in sequence (refer to the attached chromatogram), the separation degree of diglyceride peak and monoglyceride peak should meet the requirements, and the diglyceride peak and triglyceride peak should meet the requirements.
The degree of separation shall not be less than 1.
0
.
Determination method Take 0.
2g of this product, accurately weigh it, put it in a weighed 25ml volumetric flask, add 5.
0ml of tetrahydrofuran, slightly heat it in a 35°C water bath, shake to dissolve, take it out, and weigh it as the test solution , accurately measure 40 μl and inject it into the liquid chromatograph, and record the chromatogram; another appropriate amount of the reference substance of glyceryl behenate is taken, accurately weighed, dissolved in tetrahydrofuran and quantitatively diluted to make a solution containing about 40 mg per 1 ml, and the same method is used for determination.
.
Calculate the content of free glycerol, monoglyceride, diglyceride and triglyceride in the test solution according to the following formula
.
In the formula, A is the measurement result under the item of free glycerol, %; B is the measurement result under the moisture item, %; D is the calculation result of free fatty acid; 340.
58 is the molecular weight of behenic acid; 56.
11 is the molecular weight of potassium hydroxide; X is the test solution The sum of the peak areas of monoglycerides and free fatty acids; Y is the peak area of diglycerides in the test solution; Z is the peak area of triglycerides in the test solution
.
【Category】Pharmaceutical excipients, lubricants and release blockers,
etc.
【Storage】Keep tightly closed
.
