CN104154713A - Lamiophlomis freeze-drying method - Google Patents

Lamiophlomis freeze-drying method Download PDF

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Publication number
CN104154713A
CN104154713A CN201410418687.0A CN201410418687A CN104154713A CN 104154713 A CN104154713 A CN 104154713A CN 201410418687 A CN201410418687 A CN 201410418687A CN 104154713 A CN104154713 A CN 104154713A
Authority
CN
China
Prior art keywords
freeze
drying
lamiophlomis
lamiophlomis rotata
controlled
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201410418687.0A
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Chinese (zh)
Inventor
周长征
张逸霏
方方
张梅雪
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Jinan Kangzhong Pharmaceutical Research and Development Co Ltd
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Jinan Kangzhong Pharmaceutical Research and Development Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
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Publication date
Application filed by Jinan Kangzhong Pharmaceutical Research and Development Co Ltd filed Critical Jinan Kangzhong Pharmaceutical Research and Development Co Ltd
Priority to CN201410418687.0A priority Critical patent/CN104154713A/en
Publication of CN104154713A publication Critical patent/CN104154713A/en
Pending legal-status Critical Current

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Abstract

The invention relates to a lamiophlomis freeze-drying method. The lamiophlomis freeze-drying method is characterized in that lamiophlomis is freeze-dried to be with water content below 5%. The lamiophlomis prepared according to the method is stable in quality.

Description

A kind of freeze drying process of lamiophlomis rotata
Invention field
The present invention relates to medicine method for making, particularly a kind of freeze drying process of lamiophlomis rotata, belongs to medical technical field.
Background technology
Lamiophlomis rotata is the dry aerial parts of Labiatae lamiophlomis rotata platymiscium lamiophlomis rotata.It has promoting blood circulation and hemostasis, the effect of wind-expelling pain-stopping, and for traumatic injury, traumatism and bleeding, arthralgia due to wind-dampness, grasserie etc.Mainly contain the active ingredients such as flavonoids, iridoids, saponins.
Traditional Chinese medicine drying has very long history in China, the Chinese herbal medicine of drying can keep certain medicinal ingredient and be difficult for putrid and deteriorated, the dry important measures as guaranteeing Chinese herbal medicine quality, it is a requisite technical process in Chinese herbal medicine processing, it is in close relations that dry and Chinese medicine are produced, and dry method will directly affect the quality of product.
Chinese pharmacopoeia version in 2010, stipulates under lamiophlomis rotata check item, moisture must not cross 13.0%.Lamiophlomis rotata medicinal material moisture content is how many, and guarantee quality of medicinal material is stable, and existing document is report not.
Summary of the invention
The freeze drying process that the object of this invention is to provide a kind of lamiophlomis rotata, the lamiophlomis rotata of the method freeze-drying, quality of medicinal material is stable.
The present invention is achieved in that
A freeze drying process for lamiophlomis rotata, freeze-drying to moisture below 5%.
The freeze drying process of a kind of lamiophlomis rotata of the present invention, solidification point is controlled at below-10 ℃, reaches and controls after temperature, is evacuated to below drying chamber pressure 30Pa heating sublimation; Sublimation temperature is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, freeze-drying to moisture below 5%.
The freeze drying process of a kind of lamiophlomis rotata of the present invention, freeze-drying to moisture below 5%, judgement by the following method, when the vacuum valve of closing between freeze drying box and condenser, hothouse internal pressure rises and to finish freeze-drying while being less than 1.5Pa in lmin internal pressure.
So far completed the present invention, lamiophlomis rotata quality of medicinal material prepared by the present invention is stable.
Below by test example, further illustrate usefulness of the present invention, test example is intended to further illustrate usefulness of the present invention, but not limitation of the present invention.
Freeze-drying lamiophlomis rotata by water content 3%, 5%, 7%, 10%, 13%, was deposited in general MED DEP, respectively at 1,2,3,6,12 month mensuration test sample general flavone content (in dry product).
4, result of the test: result of the test is in Table 1.
Table 1 different moisture content freeze-drying lamiophlomis rotata quality stability is investigated result
? 0 month 1 month 2 months 3 months 6 months 12 months
Water content 3% 6.32 6.32 6.33 6.32 6.32 6.32
Water content 5% 6.33 6.34 6.33 6.32 6.33 6.34
Water content 7% 6.31 6.32 6.27 6.15 6.0 5.98
Water content 10% 6.32 6.30 6.24 6.19 5.72 5.15
Water content 13% 6.33 6.27 6.18 5.90 5.38 5.0
By table 1, found out, freeze-drying lamiophlomis rotata water content below 5% at general MED DEP, quality is more stable.
The specific embodiment
embodiment 1
Get fresh lamiophlomis rotata, put in freeze dryer, be refrigerated to-20 ℃, be evacuated to drying chamber pressure 30Pa, heating sublimation, the temperature of distillation is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, when the vacuum valve of closing between freeze drying box and condenser, hothouse internal pressure finishes when the rising of lmin internal pressure is less than 1.5Pa.Through chemical examination, lamiophlomis rotata moisture 5%.
embodiment 2
Get fresh lamiophlomis rotata, pile vexed 2 days, put in freeze dryer, be refrigerated to-28 ℃, be evacuated to drying chamber pressure 50Pa, heating sublimation, the temperature of distillation is controlled at 50 ℃, resolution temperature is controlled at below 45 ℃, and when the vacuum valve of closing between freeze drying box and condenser, hothouse internal pressure finishes freeze-drying when the rising of lmin internal pressure is less than 1Pa.Through chemical examination, lamiophlomis rotata moisture 3%.
embodiment 3
Get fresh lamiophlomis rotata, pile vexed 2 days, put in freeze dryer, put in freeze dryer, be refrigerated to-32 ℃, be evacuated to drying chamber pressure 50Pa, heating sublimation, the temperature of distillation is controlled at 50 ℃, and resolution temperature is controlled at below 45 ℃, when the vacuum valve of closing between freeze drying box and condenser, hothouse internal pressure finishes freeze-drying when the rising of lmin internal pressure is less than 0.5Pa.Through chemical examination, lamiophlomis rotata moisture 1%.
embodiment 4
Get fresh lamiophlomis rotata, pile vexed 5 days, put in freeze dryer, put in freeze dryer, be refrigerated to-32 ℃, be evacuated to drying chamber pressure 50Pa, heating sublimation, the temperature of distillation is controlled at 50 ℃, and resolution temperature is controlled at below 45 ℃, when the vacuum valve of closing between freeze drying box and condenser, hothouse internal pressure finishes freeze-drying when the rising of lmin internal pressure is less than 2Pa.Through chemical examination, lamiophlomis rotata is moisture 10%, defective.

Claims (2)

1. a freeze drying process for lamiophlomis rotata, is characterized in that: freeze-drying is that solidification point is controlled at below-10 ℃, reaches and controls after temperature, is evacuated to below drying chamber pressure 30Pa heating sublimation; Sublimation temperature is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, freeze-drying to moisture below 5%.
2. according to the freeze drying process of a kind of lamiophlomis rotata of claim 1, it is characterized in that: freeze-drying to moisture below 5%, judgement by the following method, when the vacuum valve of closing between freeze drying box and condenser, hothouse internal pressure finishes freeze-drying when the rising of lmin internal pressure is less than 1.5Pa.
CN201410418687.0A 2014-08-25 2014-08-25 Lamiophlomis freeze-drying method Pending CN104154713A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410418687.0A CN104154713A (en) 2014-08-25 2014-08-25 Lamiophlomis freeze-drying method

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410418687.0A CN104154713A (en) 2014-08-25 2014-08-25 Lamiophlomis freeze-drying method

Publications (1)

Publication Number Publication Date
CN104154713A true CN104154713A (en) 2014-11-19

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CN201410418687.0A Pending CN104154713A (en) 2014-08-25 2014-08-25 Lamiophlomis freeze-drying method

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Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3835550A (en) * 1972-08-21 1974-09-17 K Kaneko Freeze-drying process for producing a dry plant
FR2553873A1 (en) * 1983-10-19 1985-04-26 Allorge Lucile Method for drying, stabilising, decontaminating and de-infesting medicinal or seasoning plants using a microwave oven
CN101953805A (en) * 2010-09-29 2011-01-26 贵州益佰制药股份有限公司 Method for preparing antitumor medical preparation
CN103055096A (en) * 2013-01-10 2013-04-24 济南康众医药科技开发有限公司 Application for freeze-dried Chinese yam in medicine preparation
CN103169741A (en) * 2013-01-10 2013-06-26 济南康众医药科技开发有限公司 Application of freeze-dried portulaca oleracea L. in preparation of anti-fatigue medicament
US20130316028A1 (en) * 2011-02-15 2013-11-28 Alberta Berendina Buring Freeze dried extract of parkia, preferably of parkia speciosa beans for treatment of diseases such as diabetes mellitus type 2
CN103948652A (en) * 2014-05-15 2014-07-30 济南康众医药科技开发有限公司 Method for drying lucid ganoderma
CN103954100A (en) * 2014-05-15 2014-07-30 济南康众医药科技开发有限公司 Application of refrigeration technology in drying hericium erinaceus

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3835550A (en) * 1972-08-21 1974-09-17 K Kaneko Freeze-drying process for producing a dry plant
FR2553873A1 (en) * 1983-10-19 1985-04-26 Allorge Lucile Method for drying, stabilising, decontaminating and de-infesting medicinal or seasoning plants using a microwave oven
CN101953805A (en) * 2010-09-29 2011-01-26 贵州益佰制药股份有限公司 Method for preparing antitumor medical preparation
US20130316028A1 (en) * 2011-02-15 2013-11-28 Alberta Berendina Buring Freeze dried extract of parkia, preferably of parkia speciosa beans for treatment of diseases such as diabetes mellitus type 2
CN103055096A (en) * 2013-01-10 2013-04-24 济南康众医药科技开发有限公司 Application for freeze-dried Chinese yam in medicine preparation
CN103169741A (en) * 2013-01-10 2013-06-26 济南康众医药科技开发有限公司 Application of freeze-dried portulaca oleracea L. in preparation of anti-fatigue medicament
CN103948652A (en) * 2014-05-15 2014-07-30 济南康众医药科技开发有限公司 Method for drying lucid ganoderma
CN103954100A (en) * 2014-05-15 2014-07-30 济南康众医药科技开发有限公司 Application of refrigeration technology in drying hericium erinaceus

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
詹丽茵: "冷冻干燥技术的中药应用研究", 《中国医药导报》 *
闫家福等: "冷冻干燥技术及其在中药研究中的应用", 《中国实验方剂学杂志》 *

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Application publication date: 20141119