CN102106968A - Process for carrying out impurity removal on syrup technical extract for nourishing yin to clear away lung-heat by flocculation and subsequent separation - Google Patents
Process for carrying out impurity removal on syrup technical extract for nourishing yin to clear away lung-heat by flocculation and subsequent separation Download PDFInfo
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Abstract
The invention provides a process for carrying out impurity removal on a syrup technical extract for nourishing yin to clear away lung-heat by flocculation and subsequent separation. The process comprises the following steps: respectively adding a proper amount of ZTC1 plus 1 flocculating agent and chitosan in syrup technical water extract for nourishing yin to clear away lung-heat and alcohol extraction solution; removing impurities by flocculation under the stirring condition; after carrying out gravitational settling or centrifugal settling on the flocculated liquid medicine, filtering sediment by a filter press; combining filtrate with the settled supernate; filtering by a micro filtration membrane to obtain a clarified liquid medicine; respectively condensing the treated water extract solution and the alcohol extraction solution to be a proper amount; combining the concentrate, adding 0.3 percent sodium benzoate and uniformly stirring; and adding syrupus simplex and mint camphor, uniformly stirring, standing and filling. According to the method, most of impurities in the liquid medicine can be removed and the retaining rate of effective components and the clarity of the liquid medicine can be improved.
Description
Technical field
The preparation technology who the invention belongs to syrup for nourishing and clearing lung-heat improves, former medicament extracting solution flocculation remove impurity of particularly a kind of syrup for nourishing and clearing lung-heat and follow-up separation process.
Background technology
Syrup for nourishing and clearing lung-heat comes from the nourishing YIN and clearing away lung-heat side of Qing Dynasty's Zheng Meijian " Chonglou Yuyao, Jade Key to the Secluded Chamber ", form by Radix Rehmanniae, Radix Ophiopogonis, Radix Scrophulariae, Bulbus Fritillariae Cirrhosae, the Radix Paeoniae Alba, Cortex Moutan, Radix Glycyrrhizae, Herba Menthae eight flavor Chinese medicines, on former decoction basis, it is formulated to add a certain proportion of simple syrup.Effect with nourishing YIN and clearing away lung-heat, relieving sore-throat by clearing away heat, diseases such as the cough that causes for the deficiency of YIN, dry laryngopharynx pain, the few expectorant of dry cough, sputum mixed with blood all have significant therapeutic effect.Syrup for nourishing and clearing lung-heat is put into " Drug Standard of Ministry of Public Health of the Peoples Republic of China Chinese traditional patent formulation preparation " the 4th (WS3-B-2956-98), traditional handicraft is with twice of Radix Rehmanniae, Radix Scrophulariae, Radix Ophiopogonis, Radix Glycyrrhizae decocting in water, merge decocting liquid, be concentrated in right amount, Cortex Moutan, Bulbus Fritillariae Cirrhosae, the Radix Paeoniae Alba are used 60% ethanol extraction; Above-mentioned decocting in water concentrated solution and ethanol extract are merged mixing, leave standstill, it is standby to draw supernatant.Precipitation changes molten with an amount of 70% ethanol.Fully mixing leaves standstill, and draws supernatant, and precipitation is used with method and dissolved once again, the filtering precipitation, merge solution twice, reclaim ethanol, be concentrated in right amount, above-mentioned reserve liquid and concentrated solution are merged, add 0.3% sodium benzoate and stir evenly, add simple syrup and Mentholum and stir evenly, leave standstill fill.The alcohol deposition method that this process using is traditional is used for the purification and impurity removal of herb liquid, not only the production cycle is long, energy consumption is big, complicated operation, and when removing impurity, also heavy losses effective ingredient, and the poor stability of medicinal liquid, wall sticking phenomenon easily takes place in long-term the placement, to such an extent as to influence the clinical efficacy of preparation.
Summary of the invention
The purpose of this invention is to provide flocculation remove impurity of the former medicament extracting solution of a kind of syrup for nourishing and clearing lung-heat and follow-up separation process, can overcome the defective of prior art, with better removal impurity, keep effective ingredient, shorten the production cycle, reduce production costs.
The step that former medicament extracting solution flocculation remove impurity of a kind of syrup for nourishing and clearing lung-heat provided by the invention and follow-up separation process comprise:
1) presses syrup for nourishing and clearing lung-heat prescription former liquid medicine extract of preparation and former medicine alcohol extract.
2) under 25～40 ℃ of temperature, the ZTC1+1 flocculating agent is joined in the former liquid medicine extract of syrup for nourishing and clearing lung-heat, and the remove impurity of flocculating under stirring condition reaction is behind the medicinal liquid process gravitational settling or centrifugal sedimentation after the flocculation, sediment filters through pressure filter, and the clear liquid after filtrate and the sedimentation is merged; Through micro-filtrate membrane filtration, must clarify medicinal liquid again.
3) under 20～40 ℃ of temperature, to join in the former medicine alcohol extract of syrup for nourishing and clearing lung-heat with chitosan, the remove impurity of flocculating under stirring condition reaction is behind the medicinal liquid process gravitational settling or centrifugal sedimentation after the flocculation, sediment filters through pressure filter, and the clear liquid after filtrate and the sedimentation is merged; Through micro-filtrate membrane filtration, must clarify medicinal liquid again.
4) water extract and the alcohol extract after will handling is concentrated into respectively in right amount, merges concentrated solution, adds 0.3% sodium benzoate and stirs evenly, and adds medical formula ratio simple syrup and Mentholum again and stirs evenly, and leaves standstill fill.
Described former liquid medicine extract concentration is 0.1g crude drug/mL medicinal liquid, and the addition of ZTC1+1 flocculating agent is 0.45～0.9g/L;
Step 2) stirring condition described in the flocculation reaction adopts to stir fast earlier again and stirs at a slow speed, wherein mixing speed is controlled at 250～650r/min fast, mixing time is controlled at 60～140S fast, and mixing speed is controlled at 25～75r/min at a slow speed, and mixing time is controlled at 7～25min at a slow speed.
Step 2) the gravitational settling time of the water extract after the described flocculation was controlled at 3～5 hours, and the centrifugal rotational speed of centrifugal sedimentation is controlled at 3000～5000r/min, and the centrifugalize time is controlled at 15～30min.
The described former medicine alcohol extract concentration of step 3) is 0.12g crude drug/mL medicinal liquid, and the addition of chitosan flocculant is 0.05～0.2g/L; Adopt in the step 3) flocculation reaction to stir again fast earlier and stir at a slow speed, wherein mixing speed is controlled at 250～500r/min fast, mixing time is controlled at 30～70s fast, and mixing speed is controlled at 25～80r/min at a slow speed, and mixing time is controlled at 10～40min at a slow speed.
The gravitational settling time of the alcohol extract after the step 3) flocculation was controlled at more than 5 hours, and the centrifugal rotational speed of centrifugal sedimentation is controlled at 3000～5000r/min, and the centrifugalize time is controlled at 10～25min.
Optional filter press of described pressure filter or chamber-type press filter.Ceramic membrane or the hollow-fibre membrane of the optional 0.2 μ m of described micro-filtration membrane～2 μ m.
The present invention compares with former technology, after adopting new technology, colloid in the syrup for nourishing and clearing lung-heat original liquid, protein, tannin and other non-active ingredients are effectively removed, and the retention rate of effective ingredient has improved 25% in the former liquid medicine extract, and clarity is doubled, Protein content has reduced by 57% in the alcohol extract, clarity also obviously improves, and has guaranteed the stability of medicinal liquid simultaneously, places after one month, turbidity has only increased 3.1NTU, and the production cycle shortened to less than 7 days by original 28 days.
Description of drawings
Fig. 1 is former medicament extracting solution flocculation remove impurity of syrup for nourishing and clearing lung-heat and follow-up separation process flow chart.
The specific embodiment
Below in conjunction with example the specific embodiment of the present invention is further described.
Example 1
(1) preparation of former medicament extracting solution: in syrup for nourishing and clearing lung-heat prescription ratio in the drug standard, get Radix Rehmanniae 300g, Radix Ophiopogonis 180g, Radix Scrophulariae 240g, Radix Glycyrrhizae 60g, add water (medical material gross weight 10 times, 8 times) and decoct twice (3h, 2h), collecting decoction, filter, add water to 7800mL, getting concentration is the water extract of 0.1g crude drug/mL medicinal liquid; Get Bulbus Fritillariae Cirrhosae, the Radix Paeoniae Alba, each 120g of Cortex Moutan, add 60% ethanol of 8 times of medical material gross weights, merceration three days filters, and with rotary evaporator the ethanol in the filtrate is carried to the greatest extent, adds water to 3000mL, and getting concentration is the alcohol extract of 0.12g crude drug/mL medicinal liquid.
(2) the flocculation remove impurity and the separation of former liquid medicine extract: regulating the flocculation reaction temperature is 30 ℃, ZTC1+1 flocculating agent (ZTC-III type with 0.6g/L, Tianjin shakes day a Science and Technology Ltd. to produce) join in the former liquid medicine extract, under the 450r/min rotating speed, stir 120S fast, under the 50r/min rotating speed, stir 10min then at a slow speed.Stir to finish back standing sedimentation 1 hour, clear liquid is centrifugalize 20min under the rotating speed of 3000r/min, draws the supernatant after centrifugal, standby, merge precipitation twice, filter through filter press, merge above-mentioned standby clear liquid and filtrate,, get the primary water extract through the ceramic membrane filter of 0.5 μ m.
(3) the flocculation remove impurity and the separation of former medicine alcohol extract: regulating the flocculation reaction temperature is 20 ℃, and the chitosan of 0.125g/L is joined in the former medicine alcohol extract, stirs 1min under the 350r/min rotating speed fast, stirs 10min then under the rotating speed of 50r/min at a slow speed.Stir and finish back standing sedimentation 1 hour, clear liquid is centrifugalize 15min under the rotating speed of 3000r/min, draws centrifugal back supernatant, standby, merge precipitation twice, filter through filter press, merge above-mentioned standby clear liquid and filtrate,, must clarify alcohol extract through the ceramic membrane filter of 0.5 μ m.
(4) to be concentrated into relative density respectively be 1.20 for water extract after will handling and alcohol extract, merges concentrated solution, adds sodium benzoate by 0.3% of medicinal liquid weight and stir evenly, and adds simple syrup 1870mL again and Mentholum 0.375g stirs evenly, and leaves standstill fill.
Example 2
(1) preparation of former medicament extracting solution: with (1) in the example 1.
(2) the flocculation remove impurity and the separation of former liquid medicine extract: regulating the flocculation reaction temperature is 30 ℃, ZTC1+1 flocculating agent (ZTC-III type with 0.45g/L, Tianjin shakes day a Science and Technology Ltd. to produce) join in the former liquid medicine extract, under the 450r/min rotating speed, stir 100S fast, under the 50r/min rotating speed, stir 15min then at a slow speed.Stirred end back standing sedimentation 5 hours, and drew supernatant, precipitation is filtered through filter press, merges above-mentioned clear liquid and filtrate, through the ceramic membrane filter of 0.5 μ m, gets the primary water extract.
(3) the flocculation remove impurity and the separation of former medicine alcohol extract: regulating the flocculation reaction temperature is 25 ℃, and the chitosan of 0.1g/L is joined in the former medicine alcohol extract, stirs 40S under the 400r/min rotating speed fast, stirs 15min then under the rotating speed of 40r/min at a slow speed.Stir and finish back standing sedimentation 6 hours, draw supernatant, precipitation is filtered through filter press, merges above-mentioned clear liquid and filtrate, through the ceramic membrane filter of 0.5 μ m, must clarify alcohol extract.
(4) with (4) in the example 1.
Example 3
(1) preparation of former medicament extracting solution: with (1) in the example 1.
(2) the flocculation remove impurity and the separation of former liquid medicine extract: regulating the flocculation reaction temperature is 30 ℃, ZTC1+1 flocculating agent (ZTC-III type with 0.6g/L, Tianjin shakes day a Science and Technology Ltd. to produce) join in the former liquid medicine extract, under the 450r/min rotating speed, stir 120S fast, under the 50r/min rotating speed, stir 10min then at a slow speed.Flocculation medicinal liquid centrifugalize 25min under the rotating speed of 3500r/min drew supernatant after stirring finished, and precipitated through filter press and filtered, and merged above-mentioned clear liquid and filtrate, through the ceramic membrane filter of 0.5 μ m, got the primary water extract.
(3) the flocculation remove impurity and the separation of former medicine alcohol extract: regulating the flocculation reaction temperature is 25 ℃, and the chitosan of 0.125g/L is joined in the former medicine alcohol extract, stirs 1min under the 350r/min rotating speed fast, stirs 10min then under the rotating speed of 50r/min at a slow speed.Stir and finish back centrifugalize 20min under the rotating speed of 3500r/min, draw supernatant, precipitation is filtered through filter press, merges above-mentioned clear liquid and filtrate, through the ceramic membrane filter of 0.5 μ m, must clarify alcohol extract.
(4) with (4) in the example 1.
Example 4
(1) preparation of former medicament extracting solution: with (1) in the example 1.
(2) the flocculation remove impurity and the separation of former liquid medicine extract: regulating the flocculation reaction temperature is 20 ℃, ZTC1+1 flocculating agent (ZTC-III type with 0.45g/L, Tianjin shakes day a Science and Technology Ltd. to produce) join in the former liquid medicine extract, under the 400r/min rotating speed, stir 100S fast, under the 60r/min rotating speed, stir 15min then at a slow speed.Stirring finishes back flocculation medicinal liquid centrifugalize 25min under the rotating speed of 4000r/min is, draws supernatant, and precipitation is filtered through chamber-type press filter, merges above-mentioned clear liquid and filtrate, through the ceramic membrane filter of 1 μ m, gets the primary water extract.
(3) the flocculation remove impurity and the separation of former medicine alcohol extract: regulating the flocculation reaction temperature is 20 ℃, and the chitosan of 0.05g/L is joined in the former medicine alcohol extract, stirs 40s under the 300r/min rotating speed fast, stirs 15min then under the rotating speed of 40r/min at a slow speed.Stir and finish back flocculation medicinal liquid centrifugalize 15min under the rotating speed of 3000r/min, draw supernatant, precipitation is filtered through chamber-type press filter, merges above-mentioned clear liquid and filtrate, through the ceramic membrane filter of 1 μ m, must clarify alcohol extract.
(4) with (4) in the example 1.
Example 5
(1) preparation of former medicament extracting solution: with (1) in the example 1.
(2) the flocculation remove impurity and the separation of former liquid medicine extract: regulating the flocculation reaction temperature is 35 ℃, ZTC1+1 flocculating agent (ZTC-III type with 0.75g/L, Tianjin shakes day a Science and Technology Ltd. to produce) join in the former liquid medicine extract, under the 500r/min rotating speed, stir 2min fast, under the 70r/min rotating speed, stir 15min then at a slow speed.Flocculation medicinal liquid centrifugalize 30min under the rotating speed of 5000r/min drew supernatant after stirring finished, and precipitated through chamber-type press filter and filtered, and merged above-mentioned clear liquid and filtrate, through the ceramic membrane filter of 0.2 μ m, got the primary water extract.
(3) the flocculation remove impurity and the separation of former medicine alcohol extract: regulating the flocculation reaction temperature is 40 ℃, and the chitosan of 0.15g/L is joined in the former medicine alcohol extract, stirs 1min under the 500r/min rotating speed fast, stirs 15min then under the rotating speed of 60r/min at a slow speed.Stir and finish back flocculation medicinal liquid centrifugalize 20min under the rotating speed of 5000r/min, draw supernatant, precipitation is filtered through chamber-type press filter, merges above-mentioned clear liquid and filtrate, through the ceramic membrane filter of 0.2 μ m, must clarify alcohol extract.
(4) with (4) in the example 1.
Claims (9)
1. former medicament extracting solution flocculation remove impurity of a syrup for nourishing and clearing lung-heat and follow-up separation process is characterized in that the step that comprises:
1) presses syrup for nourishing and clearing lung-heat prescription former liquid medicine extract of preparation and former medicine alcohol extract;
2) under 25～40 ℃ of temperature, the ZTC1+1 flocculating agent is joined in the former liquid medicine extract of syrup for nourishing and clearing lung-heat, and the remove impurity of flocculating under stirring condition reaction is behind the medicinal liquid process gravitational settling or centrifugal sedimentation after the flocculation, sediment filters through pressure filter, and the clear liquid after filtrate and the sedimentation is merged; Through micro-filtrate membrane filtration, must clarify medicinal liquid again;
3) under 20～40 ℃ of temperature, to join in the former medicine alcohol extract of syrup for nourishing and clearing lung-heat with chitosan, the remove impurity of flocculating under stirring condition reaction is behind the medicinal liquid process gravitational settling or centrifugal sedimentation after the flocculation, sediment filters through pressure filter, and the clear liquid after filtrate and the sedimentation is merged; Through micro-filtrate membrane filtration, must clarify medicinal liquid again;
4) water extract and the alcohol extract after will handling is concentrated into respectively in right amount, merges concentrated solution, adds 0.3% sodium benzoate and stirs evenly, and adds medical formula ratio simple syrup and Mentholum again and stirs evenly, and leaves standstill fill.
2. flocculation remove impurity according to claim 1 and follow-up separation process is characterized in that described former liquid medicine extract concentration is 0.1g crude drug/mL medicinal liquid, and the addition of ZTC1+1 flocculating agent is 0.45～0.9g/L.
3. flocculation remove impurity according to claim 1 and follow-up separation process, it is characterized in that step 2) stirring condition described in the flocculation reaction adopts to stir fast earlier again and stirs at a slow speed, wherein mixing speed is controlled at 250～650r/min fast, mixing time is controlled at 60～140S fast, mixing speed is controlled at 25～75r/min at a slow speed, and mixing time is controlled at 7～25min at a slow speed.
4. flocculation remove impurity according to claim 1 and follow-up separation process, it is characterized in that step 2) gravitational settling time of water extract after the described flocculation was controlled at 3～5 hours, the centrifugal rotational speed of centrifugal sedimentation is controlled at 3000～5000r/min, and the centrifugalize time is controlled at 15～30min.
5. flocculation remove impurity according to claim 1 and follow-up separation process is characterized in that the described former medicine alcohol extract concentration of step 3) is 0.12g crude drug/mL medicinal liquid, and the addition of chitosan flocculant is 0.05～0.2g/L;
6. flocculation remove impurity according to claim 1 and follow-up separation process, it is characterized in that adopting in the step 3) flocculation reaction stirring again fast earlier and stir at a slow speed, wherein mixing speed is controlled at 250～500r/min fast, mixing time is controlled at 30～70s fast, mixing speed is controlled at 25～80r/min at a slow speed, and mixing time is controlled at 10～40min at a slow speed.
7. flocculation remove impurity according to claim 1 and follow-up separation process, the gravitational settling time that it is characterized in that the alcohol extract after step 3) is flocculated was controlled at more than 5 hours, the centrifugal rotational speed of centrifugal sedimentation is controlled at 3000～5000r/min, and the centrifugalize time is controlled at 10～25min.
8. flocculation remove impurity according to claim 1 and follow-up separation process is characterized in that optional filter press of described pressure filter or chamber-type press filter.
9. flocculation remove impurity of the former medicament extracting solution of syrup for nourishing and clearing lung-heat according to claim 1 and follow-up separation process is characterized in that described micro-filtration membrane selects ceramic membrane or the hollow-fibre membrane of 0.2 μ m～2 μ m.
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| CN201010291182 | 2010-09-26 | ||
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106923310A (en) * | 2017-04-12 | 2017-07-07 | 盐城宇峰食品科技有限公司 | A kind of syrup dedicated production technology of drink |
| CN111329985A (en) * | 2020-03-31 | 2020-06-26 | 鲁南制药集团股份有限公司 | Preparation process for improving clarity of traditional Chinese medicine liquid preparation |
-
2011
- 2011-01-14 CN CN 201110007489 patent/CN102106968A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《卫生部颁药品标准（中药成方制剂第十五册）》 19981231 卫生部药典委员会 养阴清肺糖浆 152页 1-9 , 1 * |
| 《天津大学硕士论文》 20060630 刘佳佳 中药提取液絮凝除杂效果的研究 摘要、第16页、第21页 1-9 , 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106923310A (en) * | 2017-04-12 | 2017-07-07 | 盐城宇峰食品科技有限公司 | A kind of syrup dedicated production technology of drink |
| CN111329985A (en) * | 2020-03-31 | 2020-06-26 | 鲁南制药集团股份有限公司 | Preparation process for improving clarity of traditional Chinese medicine liquid preparation |
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Application publication date: 20110629 |