Preparation method of pearl layer powder-wild chrysanthemum cream powder hypotensive tablet

The technology of Zhenju Jiangya tablet and nacre powder is applied in the field of preparation of Zhenju Jiangya tablet, which can solve the problems of uneven mixing of clonidine hydrochloride, substandard content uniformity, etc., so as to improve bioavailability and increase batch size. Productivity, the effect of improving mixing uniformity

Inactive Publication Date: 2013-03-20

TIANSHENG PHARMA GROUP

2 Cites 5 Cited by

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Problems solved by technology

During the mixing process of this process method, the chrysanthemum flower paste powder is easy to wrap clonidine hy...

Abstract

The invention discloses a preparation method of a pearl layer powder-wild chrysanthemum cream powder hypotensive tablet. The preparation method comprises the following steps of 1, carrying out equivalent incremental mixing of hydrochlorothiazide and pearl layer powder to obtain mixed powder, 2, dissolving clonidine hydrochloride by ethanol having a volume concentration of 70% to obtain a solution, uniformly mixing the solution and the mixed powder obtained by the step 1, and repeatedly stirring to obtain a mixture, 3, drying the mixture obtained by the step 2 at a temperature of 40 to 60 DEG C and crushing the dried mixture into powder, 4, adding wild chrysanthemum cream powder and rutin into the powder obtained by the step 3, mixing, and carrying out granulation, and 5, carrying out tabletting and coating. Clonidine hydrochloride is dissolved by ethanol and then is uniformly mixed with hydrochlorothiazide and pearl layer powder; the mixture is dried, crushed and is uniformly mixed with wild chrysanthemum cream powder and rutin; and the mixture is processed into particles. The preparation method can effectively prevent that clonidine hydrochloride is coated by wild chrysanthemum cream powder, improve mixing uniformity and improve bioavailability of the pearl layer powder-wild chrysanthemum cream powder hypotensive tablet.

Application Domain

Organic active ingredientsDragees +3

Technology Topic

ChemistryClonidine Hydrochloride +6

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Examples

Experimental program(3)

Example Embodiment

[0034] Embodiment 1, a kind of Zhenju antihypertensive tablet (batch number: 101101, a total of 10000 tablets), the formula is:

[0035] Wild Chrysanthemum Cream Powder 1000g

[0036] Nacre Powder 1000g

[0037] Clonidine Hydrochloride 300mg

[0038] Hydrochlorothiazide 50g

[0039] Rutin 200g

[0040] Its preparation method is as follows:

[0041] (1) Mix 50.6 g of hydrochlorothiazide and 999.7 g of nacre powder in equal amounts to obtain a mixed powder;

[0042] (2) Separately take 0.295 g of clonidine hydrochloride, add 70% ethanol to dissolve, stir the obtained solution into the above mixed powder evenly, and stir repeatedly to obtain a mixture;

[0043] (3) Dry the above mixture at a temperature of 40-60 °C, pulverize it into powder in a pulverizer, and pass it through a No. 5 sieve;

[0044] (4) Add 999.8 g of wild chrysanthemum ointment powder and 200.1 g of rutin to the above-mentioned powder that has passed through the No. 5 sieve, mix and granulate;

[0045] (5) Tablet compression and coating, and the coating weight is 2% to 3% of the total weight of the preparation;

[0046] (6) Packaging.

[0047] Performance check:

[0048] (1) Weight detection

[0049] Take 20 tablets of this product, and test the weight of the Zhenju Jiangya Tablets prepared in this example according to the provisions of Part Two (Appendix I) of the 2010 edition of the Chinese Pharmacopoeia. The results are as follows:

[0050] Table 1 Weight test results of Zhenju Jiangya Tablets

[0051]

[0052] (2) Determination of clonidine hydrochloride content

[0053] Chromatographic conditions and system adaptability: use octadecyl-bonded silica gel as filler, methanol:0. Olmol/L sodium dihydrogen phosphate solution (30:70) is the mobile phase; the detection wavelength is 210nm; the flow rate is 1.0ml/min, and the theoretical plate number is not less than 2000 in terms of clonidine hydrochloride peak.

[0054] Preparation of reference solution: take clonidine hydrochloride, accurately weigh it, add mobile phase to make a solution containing 10 μg per 1 ml, that is.

[0055] Preparation of the test solution: take 10 tablets of this product, remove the film coating, accurately weigh, grind finely, accurately weigh an appropriate amount (equivalent to 120 μg of clonidine hydrochloride), place it in a 50ml measuring bottle, add citric acid- Disodium hydrogen phosphate buffer (pH 4.0) 40ml, sonicated for 40min, cooled and added citric acid-disodium hydrogen phosphate buffer (pH 4.0) to the mark, centrifuged, precision suction supernatant 25ml, precision added sodium carbonate 10ml of the test solution, 25ml of the supernatant was accurately drawn and placed in a separatory funnel, extracted with dichloromethane 3 times, 25ml of each extraction, combined with the dichloromethane extracts, placed in a warm water bath, volatilized to remove the dichloromethane, and added in portions Dilute the mobile phase to 5ml and shake well.

[0056] Determination method: Precisely draw 20 μl of the reference solution and the test solution, respectively, and inject them into a liquid chromatograph for determination. The measurement results are as follows:

[0057] Table 2 Assay results of clonidine hydrochloride content

[0058]

[0059] (3) Content uniformity detection of clonidine hydrochloride

[0060] Take 10 pieces of this product, remove the film coating, grind each piece in a mortar, wash in a 25ml volumetric flask, add 20ml of citric acid-disodium hydrogen phosphate buffer (pH4.0), ultrasonicate for 40min, cool and add Citric acid-disodium hydrogen phosphate buffer (pH4.0) to the mark, centrifuged, precision suction supernatant 20ml, precision add sodium carbonate test solution 10ml, mix, centrifuge, precision suction supernatant 20ml and place in a separatory funnel , extract 3 times with dichloromethane, 25ml each time, combine the dichloromethane extracts, put them in a warm water bath, volatilize to remove the dichloromethane, add the mobile phase to 5ml in stages, shake well, and use as the test solution . According to the content determination method, the test results are as follows:

[0061] Table 3 Clonidine hydrochloride content uniformity test results

[0062]

[0063] (4) Analysis of results

[0064] The content of clonidine hydrochloride in Zhenju Jiangya Tablets produced in this example is 94.8%, and the A+1.80S value of clonidine hydrochloride is 12.5, all of which meet the relevant requirements of the 2010 edition of the Chinese Pharmacopoeia.

Example Embodiment

[0065] Embodiment 2, a kind of Zhenju Jiangya tablet (batch number: 101102, a total of 10000 tablets), the formula is:

[0066] Wild Chrysanthemum Cream Powder 1000g

[0067] Nacre Powder 1000g

[0068] Clonidine Hydrochloride 300mg

[0069] Hydrochlorothiazide 50g

[0070] Rutin 200g

[0071] Its preparation method is as follows:

[0072] (1) Take the mixed powder of 50.7g hydrochlorothiazide and 1000.1g nacre powder mixed in equal amounts;

[0073] (2) Separately take 0.312 g of clonidine hydrochloride, add 70% ethanol to dissolve it, stir the obtained solution into the above mixed powder evenly, and stir the mixture repeatedly;

[0074] (3) Dry the above mixture at a temperature of 40-60 °C, and pulverize it into powder in a pulverizer;

[0075] (4) Add 1000.1 g of wild chrysanthemum ointment powder and 200.1 g of rutin to the above-mentioned pulverized powder, mix and granulate;

[0076] (5) Compress into 10,000 tablets, and coat the compressed tablets, and the weight of the coating is 2% to 3% of the total weight of the preparation;

[0077] (6) Packaging.

[0078] Performance measurement:

[0079] (1) Weight detection

[0080] Take 20 tablets of this product, and test the weight of Zhenju Jiangya Tablets prepared in this example according to the provisions of "Chinese Pharmacopoeia" (2010 Edition) , and the results are as follows:

[0081] Table 4 Weight test results of Zhenju Jiangya Tablets

[0082]

[0083] (2) Determination of clonidine hydrochloride content

[0084] Chromatographic conditions and system adaptability: use octadecyl-bonded silica gel as filler, methanol:0. Olmol/L sodium dihydrogen phosphate solution (30:70) is the mobile phase; the detection wavelength is 210nm;

[0085] Preparation of reference substance solution: Take an appropriate amount of clonidine hydrochloride reference substance and accurately weigh it. Add mobile phase to make a solution containing 10 μg per 1 ml, that is.

[0086] Preparation of the test solution: take 10 tablets of this product, remove the film coating, accurately weigh, grind finely, accurately weigh an appropriate amount (equivalent to 120 μg of clonidine hydrochloride), place it in a 50ml measuring bottle, add citric acid- Disodium hydrogen phosphate buffer (pH 4.0) 40ml, sonicated for 40min, cooled and added citric acid-disodium hydrogen phosphate buffer (pH 4.0) to the mark, centrifuged, precision suction supernatant 25ml, precision added sodium carbonate 10ml of the test solution, 25ml of the supernatant was accurately drawn into a separatory funnel, extracted three times with dichloromethane, 25ml each time, combined with the dichloromethane extracts, placed in a warm water bath, volatilized to remove the dichloromethane, and added in several times Dilute the mobile phase to 5ml,

[0087] Shake well and you're done.

[0088] Determination method: Precisely draw 20 μl of the reference solution and the test solution, respectively, and inject them into a liquid chromatograph for determination. The measurement results are as follows

[0089] Table 5 Determination results of clonidine hydrochloride content

[0090]

[0091] (3) Content uniformity detection of clonidine hydrochloride

[0092] Take 10 pieces of this product, remove the film coating, grind each piece in a mortar, wash in a 25ml volumetric flask, add 20ml of citric acid-disodium hydrogen phosphate buffer (pH4.0), ultrasonicate for 40min, cool and add Citric acid-disodium hydrogen phosphate buffer (pH4.0) to the mark, centrifuged, precision suction supernatant 20ml, precision add sodium carbonate test solution 10ml, mix, centrifuge, precision suction supernatant 20ml and place in a separatory funnel , extract 3 times with dichloromethane, each 25ml, combine the dichloromethane extracts, put them in a warm water bath, volatilize and remove the dichloromethane, add the mobile phase in several times to make up to 5ml, shake well, and use it as the test solution. According to the content determination method, the results are as follows:

[0093] Table 6 Clonidine Hydrochloride Content Uniformity Determination Results

[0094]

[0095] (4) Analysis of results

[0096] The content of clonidine hydrochloride in Zhenju Jiangya Tablets in this example is 94.6%, and the A+1.80S value of clonidine hydrochloride is 11.4, which all meet the relevant requirements of the 2010 edition of the Chinese Pharmacopoeia.

Example Embodiment

[0097] Embodiment 3, a kind of Zhenju antihypertensive tablet (batch number: 101103, a total of 10000 tablets), the formula is:

[0098] Wild Chrysanthemum Cream Powder 1000g

[0099] Nacre Powder 1000g

[0100] Clonidine Hydrochloride 300mg

[0101] Hydrochlorothiazide 50g

[0102] Rutin 200g

[0103] The preparation method is as follows:

[0104] (1) Take the mixed powder of 49.9g hydrochlorothiazide and 1000.4g nacre powder mixed in equal amounts;

[0105] (2) Separately take 0.312 g of clonidine hydrochloride, add 70% ethanol to dissolve it, stir the obtained solution into the above mixed powder evenly, and stir the mixture repeatedly;

[0106] (3) Dry the above mixture at a temperature of 40-60 °C, and pulverize it into powder in a pulverizer;

[0107] (4) Add 1000.1 g of wild chrysanthemum ointment powder and 299.9 g of rutin to the above crushed powder, mix and granulate;

[0108] (5) Tablet compression and coating, and the coating weight is 2% to 3% of the total weight of the preparation;

[0109] (6) Packaging.

[0110] Performance measurement:

[0111] (1) Weight detection

[0112] Take 20 tablets of this product, and test the weight of Zhenju Jiangya Tablets prepared in this example according to the provisions of "Chinese Pharmacopoeia" (2010 edition) , and the results are as follows:

[0113] Table 7 Weight test results of Zhenju Jiangya Tablets

[0114]

[0115] (2) Determination of clonidine hydrochloride content

[0116] Chromatographic conditions and system adaptability: use octadecyl-bonded silica gel as filler, methanol:0. Olmol/L sodium dihydrogen phosphate solution (30:70) is the mobile phase; the detection wavelength is 210nm;

[0117] Preparation of reference substance solution: Take an appropriate amount of clonidine hydrochloride reference substance and accurately weigh it. Add mobile phase to make a solution containing 10 μg per 1 ml, that is.

[0118]Preparation of the test solution: take 10 tablets of this product, remove the film coating, accurately weigh, grind finely, accurately weigh an appropriate amount (equivalent to 120 μg of clonidine hydrochloride), place it in a 50ml measuring bottle, add citric acid- Disodium hydrogen phosphate buffer (pH 4.0) 40ml, sonicated for 40min, cooled and added citric acid-disodium hydrogen phosphate buffer (pH 4.0) to the mark, centrifuged, precision suction supernatant 25ml, precision added sodium carbonate 10ml of the test solution, 25ml of the supernatant was accurately drawn into a separatory funnel, extracted three times with dichloromethane, 25ml each time, combined with the dichloromethane extracts, placed in a warm water bath, volatilized to remove the dichloromethane, and added in several times Dilute the mobile phase to 5ml,

[0119] Shake well and you're done.

[0120] Determination method: Precisely draw 20 μl of the reference solution and the test solution, respectively, and inject them into a liquid chromatograph for determination. The measurement results are shown in the table below:

[0121] Table 8 Determination results of clonidine hydrochloride content

[0122]

[0123] (3) Content uniformity detection of clonidine hydrochloride

[0124] Take 10 pieces of this product, remove the film coating, grind each piece in a mortar, wash in a 25ml volumetric flask, add 20ml of citric acid-disodium hydrogen phosphate buffer (pH4.0), ultrasonicate for 40min, cool and add Citric acid-disodium hydrogen phosphate buffer (pH4.0) to the mark, centrifuged, precision suction supernatant 20ml, precision add sodium carbonate test solution 10ml, mix, centrifuge, precision suction supernatant 20ml and place in a separatory funnel , extract 3 times with dichloromethane, each extraction 25ml, combine the dichloromethane extracts, put them in a warm water bath, volatilize and remove the dichloromethane, add the mobile phase in several times to make up to 5ml, shake well, as the test solution . According to the content determination method. The measurement results are as follows:

[0125] Table 9 Determination results of clonidine hydrochloride content uniformity

[0126]

[0127] (4) Analysis of results

[0128] The content of clonidine hydrochloride in Zhenju Jiangya Tablets in this example is 95.9%, the A+1.80S value of clonidine hydrochloride is 11.0, and the content and uniformity of clonidine hydrochloride meet the relevant requirements of the 2010 edition of the Chinese Pharmacopoeia.

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Preparation method of pearl layer powder-wild chrysanthemum cream powder hypotensive tablet

AI-Extracted Technical Summary

Problems solved by technology

Abstract

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Examples

Example Embodiment

Example Embodiment

Example Embodiment

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Description & Claims & Application Information

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