CN107638383A - The preparation technology of penehyclidine hydrochloride injection - Google Patents
The preparation technology of penehyclidine hydrochloride injection Download PDFInfo
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- CN107638383A CN107638383A CN201610575233.3A CN201610575233A CN107638383A CN 107638383 A CN107638383 A CN 107638383A CN 201610575233 A CN201610575233 A CN 201610575233A CN 107638383 A CN107638383 A CN 107638383A
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Abstract
The invention discloses a kind of preparation technology of penehyclidine hydrochloride injection, belong to medical drugses field.The specific preparation flow of the parenteral solution is：（1）Interior packaging material ampoule bottle or cillin bottle are placed 0.5 ~ 1 hour through the immersion of 60 120 DEG C of drinking water in advance, then rear high temperature sterilization drying for standby is washed with water in purified water, parenteral solution；（2）Amyl ethyl quin ether hydrochloride is weighed by recipe quantity, adds appropriate water for injection to make dissolving, then is added to the full amount of water for injection, is stirred evenly；（3）Filtering, embedding high-temperature sterilization, produce in standby interior packaging material.The penehyclidine hydrochloride injection product obtained by the process is more stable in terms of pH, content, visible foreign matters, more without allogenic material.
Description
Technical field
The present invention relates to a kind of preparation method of injection decoction, and in particular to selective anticholinergic agent amyl ethyl quin ether hydrochloride
A kind of preparation technology of parenteral solution, belongs to medical drugses field.
Technical background
It is as follows by the retrieval to penehyclidine hydrochloride injection Patents, its present situation：Penehyclidine hydrochloride injection
In preparation process the patent CN102525909B that pH value is 4.6-4.8 is adjusted with aqueous hydrochloric acid solution.Interior packaging material ampoule bottle or west
Woods bottle is with the patent CN102525910B used after HCl treatment.
Demonstrate amyl ethyl quin ether hydrochloride compound and be dissolved in water, then it is directly filling in existing any commercially available without pre-treatment
In ampoule bottle and cillin bottle, stability is bad, and long-term placement the significant change that pH value rises and content declines occurs after 6 months,
PH value and changes of contents cause drug quality and curative effect unstable, or even can exceed qualified limit, turn into unqualified medicine.
The content of the invention
Present invention seek to address that existing penehyclidine hydrochloride injection is in without the commercially available ampoule bottle of any processing and XiLin
Stability is bad in bottle, and long-term placement pH value occurs after 6 months and rises the problem of declining with content, there is provided a kind of second Kui of hydrochloric acid penta
The novel preparation process of ether parenteral solution, internally packaging material is handled in advance especially before to penehyclidine hydrochloride injection embedding
Method.The penehyclidine hydrochloride injection product obtained by the process is more steady in terms of pH, content, visible foreign matters
Fixed, product quality is easier to be guaranteed.
The concrete technical scheme of the present invention is as follows：
A kind of preparation technology of penehyclidine hydrochloride injection, it is characterised in that：It is pre- before penehyclidine hydrochloride injection bottling
After first internal packaging material --- ampoule bottle or cillin bottle carry out immersion treatment with 60-120 DEG C of drinking water, then by the second Kui of hydrochloric acid penta
Ether medicine liquid irrigation is encapsulated in standby interior packaging material, high-temperature sterilization, is produced.
The mode that the interior packaging material carries out water immersion treatment is：Interior packaging material is filled to 60-120 DEG C of drinking water, immersion is put
Dried after setting to 0 .5 ~ 1 hour, then purified water, parenteral solution are washed with water rear high temperature sterilization and dried, it is standby.
The preparation method of the amyl ethyl quin ether hydrochloride decoction is：Amyl ethyl quin ether hydrochloride is weighed by recipe quantity, adds appropriate injection
Make dissolving with water, then add to the full amount of water for injection, stir evenly；Then measure pH value, content, qualified rear 0.22 μm of membrane filtration,
Produce.
The specific preparation process of the penehyclidine hydrochloride injection is as follows：
Interior packaging material ampoule bottle or cillin bottle are filled to 60-120 DEG C of drinking water, immersion dries after placing 0.5 ~ 1 hour, then passes through A,
Rear high temperature sterilization drying for standby is washed with water in purified water, parenteral solution；
B, amyl ethyl quin ether hydrochloride 2.0g is weighed, adds 1600ml waters for injection to dissolve, then is added to the full amount of water for injection, stirs evenly, obtains pH
4.5 ~ 6.5, the decoction of content 90% ~ 110%；The content is labelled amount；
C, decoction embedding after 0.22 μm of membrane filtration in above-mentioned standby ampoule bottle or cillin bottle, high-temperature sterilization, produces.
Described high temperature sterilization is dry, high-temperature sterilization is pharmaceutical industry parenteral solution conventional production process, wherein：High-temperature sterilization
Preferred value：Temperature is 121 DEG C, and the time is 12 minutes.
The advantageous effects of the present invention are shown：
1st, place of --- -- the domestic small-volume injection manufacturer for interior packaging material ampoule bottle and cillin bottle relative to prior art
Reason is drying/drying after bottle washing machine is successively washed with purified water, water for injection, then the work of sterilization is dried by high temp tunnel
Skill step, the present invention are to dry this after the drinking water immersion 0.5-1 hours with 60-120 DEG C are added before above-mentioned processing
Process, internal packaging material can be passed through（Ampoule bottle or cillin bottle）After being handled with the drinking water of different temperatures, then by hydrochloric acid
Amyl ethyl quin ether medicine liquid irrigation is encapsulated in the penehyclidine hydrochloride injection obtained in standby interior packaging material, and its stability is improved significantly,
Long-term place is not in that pH value rises and the problem of content declines so that penehyclidine hydrochloride injection product in pH, contain
It is more stable in terms of amount, allogenic material is occurred without in process of production, is not in patent CN102525909B and patent
CN102525910B external sources hydrochloric acid adds to be likely to occur produces now unknown chemical reaction with glass.
2nd, the penehyclidine hydrochloride injection obtained by preparation technology of the present invention, its pH value is placed for a long time and remains to be maintained at
In 4.5 ~ 6.5 acceptability limit；Content can also be stablized in 90% ~ 110% acceptability limit simultaneously.
3rd, because the present invention takes the drinking water immersion way of specified temp, the control of passage time and temperature, so as to real
Now ensure the purpose of penehyclidine hydrochloride injection stability.
The present invention is further illustrated below in conjunction with experiment：
Test 1 prescription：Amyl ethyl quin ether hydrochloride 2g
Water for injection adds to 2000ml
（Specification：1ml∶1mg）
Preparation technology：
1. interior packaging material ampoule bottle to be filled to 60 DEG C of drinking water, dried after placing 0.5 hour, then purified water, parenteral solution water
High temperature sterilization drying for standby after washing；
2. weighing amyl ethyl quin ether hydrochloride 2.0g, add 1600ml waters for injection to dissolve, then add to the full amount of water for injection, survey pH=5.53,
Content=99.9%.Decoction after 0.22 μm of membrane filtration embedding in clean sterilizing-drying ampoule bottle in.The sample that embedding obtains
Under acceleration conditions（40℃±2℃）Place and investigate, periodically sampling detection pH value, content and visible foreign matters.
Test 2 prescriptions：Amyl ethyl quin ether hydrochloride 2g
Water for injection adds to 2000ml
（Specification：1ml∶1mg）
Preparation technology：
1. interior packaging material ampoule bottle to be filled to 80 DEG C of drinking water, dried after placing 0.5 hour, then purified water, parenteral solution water
High temperature sterilization drying for standby after washing；
2. weighing amyl ethyl quin ether hydrochloride 2.0g, add 1600ml waters for injection to dissolve, then add to the full amount of water for injection, survey pH=5.48,
Content=99.6%.Decoction after 0.22 μm of membrane filtration embedding in clean sterilizing-drying ampoule bottle in.The sample that embedding obtains
Under acceleration conditions（40℃±2℃）Place and investigate, periodically sampling detection pH value, content and visible foreign matters.
Test 3 prescriptions：Amyl ethyl quin ether hydrochloride 2g
Water for injection adds to 2000ml
（Specification：1ml∶1mg）
Preparation technology：
1. interior packaging material ampoule bottle to be filled to 100 DEG C of drinking water, dried after placing 0.5 hour, then purified water, parenteral solution water
High temperature sterilization drying for standby after washing；
2. weighing amyl ethyl quin ether hydrochloride 2.0g, add 1600ml waters for injection to dissolve, then add to the full amount of water for injection, survey pH=5.52,
Content=99.5%.Decoction after 0.22 μm of membrane filtration embedding in clean sterilizing-drying ampoule bottle in.The sample that embedding obtains
Under acceleration conditions（40℃±2℃）Place and investigate, periodically sampling detection pH value, content and visible foreign matters.
Test 4 prescriptions：Amyl ethyl quin ether hydrochloride 2g
Water for injection adds to 2000ml
（Specification：1ml∶1mg）
Preparation technology：
1. interior packaging material ampoule bottle to be filled to 120 DEG C of drinking water, dried after placing 0.5 hour, then purified water, parenteral solution water
High temperature sterilization drying for standby after washing；
2. weighing amyl ethyl quin ether hydrochloride 2.0g, add 1600ml waters for injection to dissolve, then add to the full amount of water for injection, survey pH=5.45,
Content=99.7%.Decoction after 0.22 μm of membrane filtration embedding in clean sterilizing-drying ampoule bottle in.The sample that embedding obtains
Under acceleration conditions（40℃±2℃）Place and investigate, periodically sampling detection pH value, content and visible foreign matters.
Test 5 prescriptions：Amyl ethyl quin ether hydrochloride 2g
Water for injection adds to 2000ml
（Specification：1ml∶1mg）
Preparation technology：
1. interior packaging material ampoule bottle to be filled to 60 DEG C of drinking water, dried after placing 1 hour, then purified water, parenteral solution are washed with water
Wash rear high temperature sterilization drying for standby；
2. weighing amyl ethyl quin ether hydrochloride 2.0g, add 1600ml waters for injection to dissolve, then add to the full amount of water for injection, survey pH=5.56,
Content=99.9%.Decoction after 0.22 μm of membrane filtration embedding in clean sterilizing-drying ampoule bottle in.The sample that embedding obtains
Under acceleration conditions（40℃±2℃）Place and investigate, periodically sampling detection pH value, content and visible foreign matters.
Test 6 prescriptions：Amyl ethyl quin ether hydrochloride 2g
Water for injection adds to 2000ml
（Specification：1ml∶1mg）
Preparation technology：
1. interior packaging material ampoule bottle to be filled to 80 DEG C of drinking water, dried after placing 1 hour, then purified water, parenteral solution are washed with water
Wash rear high temperature sterilization drying for standby；
2. weighing amyl ethyl quin ether hydrochloride 2.0g, add 1600ml waters for injection to dissolve, then add to the full amount of water for injection, survey pH=5.51,
Content=99.6%.Decoction after 0.22 μm of membrane filtration embedding in clean sterilizing-drying ampoule bottle in.The sample that embedding obtains
Under acceleration conditions（40℃±2℃）Place and investigate, periodically sampling detection pH value, content and visible foreign matters.
Test 7 prescriptions：Amyl ethyl quin ether hydrochloride 2g
Water for injection adds to 2000ml
（Specification：1ml∶1mg）
Preparation technology：
1. interior packaging material ampoule bottle to be filled to 100 DEG C of drinking water, dried after placing 1 hour, then purified water, parenteral solution are washed with water
Wash rear high temperature sterilization drying for standby；
2. weighing amyl ethyl quin ether hydrochloride 2.0g, add 1600ml waters for injection to dissolve, then add to the full amount of water for injection, survey pH=5.49,
Content=99.4%.Decoction after 0.22 μm of membrane filtration embedding in clean sterilizing-drying ampoule bottle in.The sample that embedding obtains
Under acceleration conditions（40℃±2℃）Place and investigate, periodically sampling detection pH value, content and visible foreign matters.
Test 8 prescriptions：Amyl ethyl quin ether hydrochloride 2g
Water for injection adds to 2000ml
（Specification：1ml∶1mg）
Preparation technology：
1. interior packaging material ampoule bottle to be filled to 12 DEG C of drinking water, dried after placing 1 hour, then purified water, parenteral solution are washed with water
Wash rear high temperature sterilization drying for standby；
2. weighing amyl ethyl quin ether hydrochloride 2.0g, add 1600ml waters for injection to dissolve, then add to the full amount of water for injection, survey pH=5.50,
Content=99.8%.Decoction after 0.22 μm of membrane filtration embedding in clean sterilizing-drying ampoule bottle
In.The sample that embedding obtains is under acceleration conditions（40℃±2℃）Place investigate, periodically sampling detection pH value, content and
Visible foreign matters.
Investigation the results are shown in TableTest 1-8 study on the stability results
Annotation：PH value acceptability limit is 4.5-6.5；Content acceptability limit is 90%-the 110% of labelled amount.Visible foreign matters foundation
《Chinese Pharmacopoeia》（Version four in 2015）0904 visible foreign matters inspection technique inspection.
As a result：Penehyclidine hydrochloride injection is filling after being handled through 60-120 DEG C of drinking water immersion 0.5-1 hours
Optimal stability in ampoule bottle or cillin bottle, pH value and content have no significant change, it is seen that foreign matter is also qualified.
Claims (2)
1. a kind of preparation technology of penehyclidine hydrochloride injection, it is characterised in that preparation process is as follows
Interior packaging material ampoule bottle or cillin bottle are filled to 60-120 DEG C of drinking water, immersion dries after placing 0.5 ~ 1 hour, then passes through A,
Rear high temperature sterilization drying for standby is washed with water in purified water, parenteral solution；
B, amyl ethyl quin ether hydrochloride 2.0g is weighed, adds 1600ml waters for injection to dissolve, then is added to the full amount of water for injection, stirs evenly, obtains pH
4.5 ~ 6.5, the decoction of content 90% ~ 110%；The content is labelled amount；
C, decoction embedding after 0.22 μm of membrane filtration in above-mentioned standby ampoule bottle or cillin bottle, high-temperature sterilization, produces；
The temperature of described high-temperature sterilization is 121 DEG C, and the time is 12 minutes.
2. the preparation technology of penehyclidine hydrochloride injection according to claim 1, it is characterised in that preparation process is as follows：
Interior packaging material ampoule bottle or cillin bottle are filled to 60-120 DEG C of drinking water, immersion dries after placing 0.5-1 hours, then passes through A,
Rear high temperature sterilization drying for standby is washed with water in purified water, parenteral solution；
B, amyl ethyl quin ether hydrochloride 2.0g is weighed, adds 1600ml waters for injection to dissolve, then is added to the full amount of water for injection, stirs evenly, obtains
PH 5.53, the decoction of content 99.9%；
C, embedding is in above-mentioned standby ampoule bottle or cillin bottle after 0.22 μm of membrane filtration for decoction, 121 DEG C, sterilizes 12 minutes,
Produce.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610575233.3A CN107638383A (en) | 2016-07-21 | 2016-07-21 | The preparation technology of penehyclidine hydrochloride injection |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610575233.3A CN107638383A (en) | 2016-07-21 | 2016-07-21 | The preparation technology of penehyclidine hydrochloride injection |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107638383A true CN107638383A (en) | 2018-01-30 |
Family
ID=61109569
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201610575233.3A Pending CN107638383A (en) | 2016-07-21 | 2016-07-21 | The preparation technology of penehyclidine hydrochloride injection |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113797092A (en) * | 2020-06-16 | 2021-12-17 | 四川远大蜀阳药业有限责任公司 | Method for stabilizing pH value and/or conductivity of small-volume glass container-contained liquid preparation |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234108A (en) * | 2007-01-30 | 2008-08-06 | 成都力思特制药股份有限公司 | Pharmaceutical composition containing (3S, 2'R)-3-(2'-hydroxy-2'-cyclopentyl-2'-phenylethoxy) quinuclidine hydrochloride and uses thereof |
| CN102525910A (en) * | 2012-02-29 | 2012-07-04 | 黄绍渊 | Process for preparing penehyclidine hydrochloride injection |
| CN102525909A (en) * | 2012-02-29 | 2012-07-04 | 黄绍渊 | Method for preparing penehyclidine hydrochloride injection |
| CN103284943A (en) * | 2012-02-29 | 2013-09-11 | 黄绍渊 | Novel method for preparing penehyclidine hydrochloride injection |
-
2016
- 2016-07-21 CN CN201610575233.3A patent/CN107638383A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101234108A (en) * | 2007-01-30 | 2008-08-06 | 成都力思特制药股份有限公司 | Pharmaceutical composition containing (3S, 2'R)-3-(2'-hydroxy-2'-cyclopentyl-2'-phenylethoxy) quinuclidine hydrochloride and uses thereof |
| CN102525910A (en) * | 2012-02-29 | 2012-07-04 | 黄绍渊 | Process for preparing penehyclidine hydrochloride injection |
| CN102525909A (en) * | 2012-02-29 | 2012-07-04 | 黄绍渊 | Method for preparing penehyclidine hydrochloride injection |
| CN103284943A (en) * | 2012-02-29 | 2013-09-11 | 黄绍渊 | Novel method for preparing penehyclidine hydrochloride injection |
Non-Patent Citations (1)
| Title |
|---|
| 杨明等: "《药剂学》", 31 August 2014, 中国医药科技出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113797092A (en) * | 2020-06-16 | 2021-12-17 | 四川远大蜀阳药业有限责任公司 | Method for stabilizing pH value and/or conductivity of small-volume glass container-contained liquid preparation |
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