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A method for refining and purifying disodium clodronate

Disodium clodronate, refining and purifying technology, applied in the field of refining and purifying medicines, can solve the problems of disodium clodronate, low solution clarity, inability to produce finished drugs, etc., and achieve product purity and solution clarity. High and large promotion and application value, easy operation effect

Active Publication Date: 2018-12-25
GUANGZHOU BAIYUNSHAN MINGXING PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the purity and solution clarity of the disodium clodronate prepared by the improved process are still low, and the content of related substances such as chloride ion, phosphorous acid, phosphoric acid and other impurities in the product is still relatively high, resulting in the partial preparation of The clodronate disodium API cannot be directly used in the production of finished drugs because it cannot meet the requirements of the new Pharmacopoeia in 2010

Method used

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  • A method for refining and purifying disodium clodronate
  • A method for refining and purifying disodium clodronate
  • A method for refining and purifying disodium clodronate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] S1: Activated carbon pretreatment

[0053] Weigh 116g of activated carbon and add it to 465ml of water for injection, boil for 15-30 minutes, filter through 3 layers of filter paper, and then wash with 23250ml of water for injection 4 times until no chloride is detected in the filtrate.

[0054] S2: EDTA treated activated carbon

[0055] Take by weighing 0.145g EDTA, dissolve it with 267ml water for injection, add above-mentioned gac, stir and soak for 2 hours, filter with 3 layers of filter paper, then wash with water for injection 4 times (each 4640ml) until there is no chloride substantially in the filtrate, and The pH value is between 6.9 and 7.0.

[0056] S3: activated carbon activation

[0057] Bake the above-mentioned treated medicinal activated carbon at 100-120°C for 4 hours, then bake at 120°C for 2 hours to activate it, and set it aside.

[0058] Wherein, the chloride inspection standard is: compared with the control solution made of standard sodium chlori...

Embodiment 2

[0068] S1: Activated carbon pretreatment

[0069] Weigh 116g of activated carbon and add it to 465ml of water for injection, boil for 15-30 minutes, filter through 3 layers of filter paper, and then wash with 18600mL of water for injection 4 times until no chloride is detected in the filtrate.

[0070] S2: EDTA treated activated carbon

[0071] Take by weighing 0.116g EDTA, dissolve it with 302ml water for injection, add above-mentioned gac, stir and soak for 2 hours, filter with 3 layers of filter paper, then wash with water for injection 4 times (each 4988ml) until there is no chloride substantially in the filtrate, and The pH value is between 6.9 and 7.0.

[0072] S3: activated carbon activation

[0073] Bake the above-mentioned treated medicinal activated carbon at 100-120°C for 4 hours, then bake at 120°C for 2 hours to activate it, and set it aside.

[0074] Among them, the chloride inspection standard is: compared with the control solution made of 6.0ml of standard s...

Embodiment 3

[0084] S1: Activated carbon pretreatment

[0085] Weigh 116g of activated carbon and add it to 465ml of water for injection, boil for 15-30 minutes, filter through 3 layers of filter paper, and then wash with 13950mL of water for injection 4 times until no chloride is detected in the filtrate.

[0086] S2: EDTA treated activated carbon

[0087] Take by weighing 0.097g EDTA, dissolve it with 325ml water for injection, add above-mentioned gac, stir and soak for 2 hours, filter with 3 layers of filter paper, then wash with water for injection 4 times (each 5220ml) until there is no chloride substantially in the filtrate, and The pH value is between 6.9 and 7.0.

[0088] S3: activated carbon activation

[0089] Bake the above-mentioned treated medicinal activated carbon at 100-120°C for 4 hours, then bake at 120°C for 2 hours to activate it, and set it aside.

[0090] Among them, the chloride inspection standard is: compared with the control solution made of 6.0ml of standard s...

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Abstract

The invention relates to a method for refining and purifying disodium clodronate. The method comprises the following steps: S1, treatment of activated carbon by EDTA: adding the activated carbon in an EDTA solution, stirring and enabling EDTA to be in full contact with the activated carbon, and then washing the activated carbon until chloride cannot be detected; S2, activation of the activated carbon: drying the activated carbon in S1 and activating the activated carbon; S3, impurity removal of the activated carbon: treating a coarse product solution of the disodium clodronate by using the activated carbon in S2, filtering, washing and controlling pH of filtrate not to exceed 3.65; and S4, crystallization and drying: adding ethanol in the filtrate of S3 while stirring, and after white crystals are separated out, standing, carrying out suction filtration and drying to obtain refined disodium clodronate. In the step S1, the mass ratio of EDTA to the activated carbon is 1:800-1,200; and in the step S4, the volume ratio of the ethanol to the filtrate is 1.08:1-2.13:1. The contents of related substances in the product refined and purified by the method provided by the invention are remarkably reduced on the premise of guaranteeing high yield, and the product has high purity and solution clarity and good stability.

Description

technical field [0001] The invention relates to the technical field of refining and purifying medicines, in particular to a method for refining and purifying disodium clodronate. Background technique [0002] Clodronate Disodium (Clodronate Disodium), its chemical name is: dichloromethylene diphosphonate disodium tetrahydrate. As a chemical drug, its indications are: (1) malignant tumor complicated with hypercalcemia; (2) bone pain caused by osteolytic cancer metastasis; (3) can avoid or delay malignant tumor osteolytic bone metastasis; ( 4) Various types of osteoporosis. Currently, clodronate disodium is available in two dosage forms, injection and capsule. As a commonly used drug for fighting bone cancer and preventing osteoporosis, the price of disodium clodronate is relatively high. [0003] The prior art mainly focuses on improving the preparation process of disodium clodronate, so as to increase the yield of disodium clodronate and reduce raw materials and productio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/42
CPCC07F9/42
Inventor 刘宏罗建明邓延秋李心花朱华司徒少金黄子健
Owner GUANGZHOU BAIYUNSHAN MINGXING PHARM CO LTD
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