CN106109673B - A kind of pharmaceutical applications of compound houttuynin syrup - Google Patents

A kind of pharmaceutical applications of compound houttuynin syrup Download PDF

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CN106109673B
CN106109673B CN201610777647.4A CN201610777647A CN106109673B CN 106109673 B CN106109673 B CN 106109673B CN 201610777647 A CN201610777647 A CN 201610777647A CN 106109673 B CN106109673 B CN 106109673B
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honeysuckle
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extracted
standby
distillation
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CN106109673A (en
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张树乘
赵伟
李翠平
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HEILONGJIANG ZHONGGUI PHARMACEUTICAL Co Ltd
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HEILONGJIANG ZHONGGUI PHARMACEUTICAL Co Ltd
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Abstract

The present invention relates to the field of Chinese medicines, and in particular to a kind of compound houttuynin syrup medicine and preparation method thereof and detection method.The medicine is by made by the raw material of following weight portion：100 weight portion of cordate houttuynia, 25 weight portion of the root of large-flowered skullcap, 25 weight portion of Radix Isatidis, 10 weight portion of the capsule of weeping forsythia, 10 weight portion of honeysuckle.Medicine of the present invention employs various extracting methods such as steam distillation is extracted, ethanol is extracted, water is extracted, and has efficiently extracted the active ingredient of medicine, has significantly improved the curative effect of medicine.

Description

A kind of pharmaceutical applications of compound houttuynin syrup
Technical field
The present invention relates to the field of Chinese medicines, and in particular to the preparation method and detection method of compound houttuynin syrup.
Background technology
Compound houttuynin syrup, is the exclusive product of applicant Heilungkiang Zhong Gui pharmaceutical Co. Ltds, with clear Effect of thermal detoxification, treatment affection of exogenous wind-heat cause have sore throat, the aspect such as acpuei pharyngitis, tonsillitis is with extraordinary Therapeutic effect.In clinical experimental research, inventor has found that compound houttuynin syrup has certain controlling to treating pancreatitis Therapeutic effect.
Compound houttuynin syrup is made up of the 5 herbal medicine raw material such as cordate houttuynia, the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, honeysuckle.It is existing Preparation method, be the preparation method for taking water extract-alcohol precipitation, patent applicant is continued many in the preparation technology to this medicine Find in the research in year, existing preparation technology has problems, such as extraction to water soluble ingredient, to volatile ingredient Extraction, be all not enough, applicant is carried out to existing preparation technology after experimental study substantial amounts of, repeatedly is carried out Improve and improve, obtained the preparation technology of the present invention, the preparation technology can obtain the more active components of the medicine, more have Beneficial to drug effect is improved, especially for pancreatitic treatment, the raising of curative effect is more significantly.
Meanwhile, present invention also offers new quality determining method, can more effectively control the quality of medicine.
The content of the invention
It is an object of the invention to provide a kind of medicine of compound houttuynin syrup.
It is a further object of the present invention to provide the preparation method of the compound houttuynin syrup medicine.
Present invention also offers the new pharmaceutical use of the compound houttuynin syrup medicine.
Present invention also offers the quality determining method of the compound houttuynin syrup medicine.
The purpose of the present invention is realized by the following manner：
A kind of compound houttuynin syrup medicine, the medicine are by made by the raw material of following weight portion：100 weight of cordate houttuynia Part, 25 weight portion of the root of large-flowered skullcap, 25 weight portion of Radix Isatidis, 10 weight portion of the capsule of weeping forsythia, 10 weight portion of honeysuckle.
Described compound houttuynin syrup medicine, the medicine are adopted and are prepared with the following method：
（1）Cordate houttuynia is taken, steam distillation extraction is carried out, Herba Houttuyniae volatile oil is therefrom extracted, it is standby；
（2）Extracting honeysuckle, is carried out steam distillation extraction, therefrom extracts volatile honeysuckle oil, standby；
（3）The aqueous solution after cordate houttuynia steam distillation is extracted is filtered, and is obtained the aqueous solution after cordate houttuynia distillation, is heated dense Contracting, obtains the concentrated liquid after cordate houttuynia distillation, standby；Retain the dregs of a decoction after cordate houttuynia steam distillation is extracted, it is standby；
（4）The aqueous solution after honeysuckle flower water steam distillation is extracted is filtered, and is obtained the aqueous solution after honeysuckle distillation, is heated dense Contracting, obtains the concentrated liquid after honeysuckle distillation, standby；Retain the dregs of a decoction after honeysuckle steam distillation is extracted, it is standby；
（5）By step（3）The dregs of a decoction, step after the steam distillation extraction of gained cordate houttuynia（4）Gained honeysuckle flower water steam Distillation extract after the dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, thereto plus 3 times amount 90% alcohol refluxs extractions it is secondary, Refluxing extraction 2 hours, merges ethanol extract every time, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, must mix Ethanol extracts concentrate, standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；
（6）By step（5）The dregs of a decoction after gained ethanol is extracted add 4 times of amount decoctings to boil three times, 2 hours every time, merge water extraction Liquid is taken, is filtered, obtain mixing aqueous extract, heating concentration obtains mixing water and extracts concentrate；
（7）By step（5）Gained mixed ethanol extracts concentrate, step（6）Gained mixing water extracts concentrate, step （3）Concentrated liquid, step after gained cordate houttuynia distillation（4）Concentrated liquid after gained honeysuckle distillation merges, and adds step Suddenly（1）Gained Herba Houttuyniae volatile oil, step（2）Gained volatile honeysuckle oil, mixes, obtains concentrated medicament；
（8）Sucrose is separately taken, simple syrup is made, step is added（7）Gained concentrated medicament, adds water, stirs evenly, and filters, filling, Obtain final product.
The quality determining method of compound houttuynin syrup medicine, the compound houttuynin syrup medicine is by following weight portion Made by raw material：
（1）Cordate houttuynia is taken, steam distillation extraction is carried out, Herba Houttuyniae volatile oil is therefrom extracted, it is standby；
（2）Extracting honeysuckle, is carried out steam distillation extraction, therefrom extracts volatile honeysuckle oil, standby；
（3）The aqueous solution after cordate houttuynia steam distillation is extracted is filtered, and is obtained the aqueous solution after cordate houttuynia distillation, is heated dense Contracting, obtains the concentrated liquid after cordate houttuynia distillation, standby；Retain the dregs of a decoction after cordate houttuynia steam distillation is extracted, it is standby；
（4）The aqueous solution after honeysuckle flower water steam distillation is extracted is filtered, and is obtained the aqueous solution after honeysuckle distillation, is heated dense Contracting, obtains the concentrated liquid after honeysuckle distillation, standby；Retain the dregs of a decoction after honeysuckle steam distillation is extracted, it is standby；
（5）By step（3）The dregs of a decoction, step after the steam distillation extraction of gained cordate houttuynia（4）Gained honeysuckle flower water steam Distillation extract after the dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, thereto plus 3 times amount 90% alcohol refluxs extractions it is secondary, Refluxing extraction 2 hours, merges ethanol extract every time, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, must mix Ethanol extracts concentrate, standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；
（6）By step（5）The dregs of a decoction after gained ethanol is extracted add 4 times of amount decoctings to boil three times, 2 hours every time, merge water extraction Liquid is taken, is filtered, obtain mixing aqueous extract, heating concentration obtains mixing water and extracts concentrate；
（7）By step（5）Gained mixed ethanol extracts concentrate, step（6）Gained mixing water extracts concentrate, step （3）Concentrated liquid, step after gained cordate houttuynia distillation（4）Concentrated liquid after gained honeysuckle distillation merges, and adds step Suddenly（1）Gained Herba Houttuyniae volatile oil, step（2）Gained volatile honeysuckle oil, mixes, obtains concentrated medicament；
（8）Sucrose is separately taken, simple syrup is made, step is added（7）Gained concentrated medicament, adds water, stirs evenly, and filters, filling, Obtain final product；
The quality testing of finger-print is carried out using following high-efficient liquid phase technique method to which：
（1）Chromatographic condition：Chromatographic column Waters Xbridge C18Post, mobile phase with acetonitrile as mobile phase A, with water as stream Dynamic phase B, gradient elution：0min to 12min, mobile phase A are linearly increasing to 30% from 15%, Mobile phase B from 85% linear decline to 70%, 12min to 45min, mobile phase A are linearly increasing to 80% from 30%, Mobile phase B from 70% linear decline to 20%, 45min extremely 55min, mobile phase A are maintained at 80%, and Mobile phase B is maintained at 20%, Detection wavelength 203nm, flow velocity 1.0mLmin-1；Column temperature 30 DEG C, 10 μ L of sampling volume；
（2）The preparation of reference substance solution：Precision weigh methyl n-nonyl ketone reference substance, β-cubebene reference substance, Different capsule of weeping forsythia cyclohexanol reference substance, puts in measuring bottle, plus methyl alcohol dissolves and be diluted to scale, obtains final product；
（3）The preparation of need testing solution：Precision measures compound houttuynin syrup, accurate to add ethanol, ultrasonic extraction, from The heart, miillpore filter filtration, takes subsequent filtrate as need testing solution, obtains final product；
（4）Determine：It is accurate to draw reference substance solution and need testing solution injection high performance liquid chromatograph, it is measured.
The quality determining method of described compound houttuynin syrup medicine, the compound houttuynin syrup medicine is by following heavy Made by the raw material of amount part：100 weight portion of cordate houttuynia, 25 weight portion of the root of large-flowered skullcap, 25 weight portion of Radix Isatidis, 10 weight portion of the capsule of weeping forsythia, gold 10 weight portion of honeysuckle flower, the compound houttuynin syrup medicine are adopted and are prepared with the following method：
（1）Cordate houttuynia is taken, steam distillation extraction is carried out, Herba Houttuyniae volatile oil is therefrom extracted, it is standby；
（2）Extracting honeysuckle, is carried out steam distillation extraction, therefrom extracts volatile honeysuckle oil, standby；
（3）The aqueous solution after cordate houttuynia steam distillation is extracted is filtered, and is obtained the aqueous solution after cordate houttuynia distillation, is heated dense Contracting, obtains the concentrated liquid after cordate houttuynia distillation, standby；Retain the dregs of a decoction after cordate houttuynia steam distillation is extracted, it is standby；
（4）The aqueous solution after honeysuckle flower water steam distillation is extracted is filtered, and is obtained the aqueous solution after honeysuckle distillation, is heated dense Contracting, obtains the concentrated liquid after honeysuckle distillation, standby；Retain the dregs of a decoction after honeysuckle steam distillation is extracted, it is standby；
（5）By step（3）The dregs of a decoction, step after the steam distillation extraction of gained cordate houttuynia（4）Gained honeysuckle flower water steam Distillation extract after the dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, thereto plus 3 times amount 90% alcohol refluxs extractions it is secondary, Refluxing extraction 2 hours, merges ethanol extract every time, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, must mix Ethanol extracts concentrate, standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；
（6）By step（5）The dregs of a decoction after gained ethanol is extracted add 4 times of amount decoctings to boil three times, 2 hours every time, merge water extraction Liquid is taken, is filtered, obtain mixing aqueous extract, heating concentration obtains mixing water and extracts concentrate；
（7）By step（5）Gained mixed ethanol extracts concentrate, step（6）Gained mixing water extracts concentrate, step （3）Concentrated liquid, step after gained cordate houttuynia distillation（4）Concentrated liquid after gained honeysuckle distillation merges, and adds step Suddenly（1）Gained Herba Houttuyniae volatile oil, step（2）Gained volatile honeysuckle oil, mixes, obtains concentrated medicament；
（8）Sucrose is separately taken, simple syrup is made, step is added（7）Gained concentrated medicament, adds water, stirs evenly, and filters, filling, Obtain final product；
The quality testing of finger-print is carried out using following high-efficient liquid phase technique method to which：
（1）Chromatographic condition：Chromatographic column Waters Xbridge C18Post, mobile phase with acetonitrile as mobile phase A, with water as stream Dynamic phase B, gradient elution：0min to 12min, mobile phase A are linearly increasing to 30% from 15%, Mobile phase B from 85% linear decline to 70%, 12min to 45min, mobile phase A are linearly increasing to 80% from 30%, Mobile phase B from 70% linear decline to 20%, 45min extremely 55min, mobile phase A are maintained at 80%, and Mobile phase B is maintained at 20%, Detection wavelength 203nm, flow velocity 1.0mLmin-1；Column temperature 30 DEG C, 10 μ L of sampling volume；
（2）The preparation of reference substance solution：Precision weighs methyl n-nonyl ketone reference substance 4.13mg, β-cubebene pair According to product 4.21mg, different capsule of weeping forsythia cyclohexanol reference substance 2.15mg, put in 10mL measuring bottles, plus methyl alcohol dissolves and be diluted to scale, obtains final product；
（3）The preparation of need testing solution：Precision measures 5 mL of compound houttuynin syrup, accurate to add 50% ethanol, 25 mL, 10 min of ultrasonic extraction, 4500 r/min are centrifuged 10 min, and 0.22 μm of miillpore filter filtration takes subsequent filtrate molten as test sample Liquid, obtains final product；
（4）Determine：It is accurate to draw reference substance solution and each 10 μ L injections high performance liquid chromatograph of need testing solution, surveyed It is fixed.
Compound houttuynin syrup medicine treats the application in pancreatitis medicine in preparation, and the compound houttuynin syrup medicine is By made by the raw material of following weight portion：100 weight portion of cordate houttuynia, 25 weight portion of the root of large-flowered skullcap, 25 weight portion of Radix Isatidis, 10 weight of the capsule of weeping forsythia Amount part, 10 weight portion of honeysuckle, the compound houttuynin syrup medicine are adopted and are prepared with the following method：
（1）Cordate houttuynia is taken, steam distillation extraction is carried out, Herba Houttuyniae volatile oil is therefrom extracted, it is standby；
（2）Extracting honeysuckle, is carried out steam distillation extraction, therefrom extracts volatile honeysuckle oil, standby；
（3）The aqueous solution after cordate houttuynia steam distillation is extracted is filtered, and is obtained the aqueous solution after cordate houttuynia distillation, is heated dense Contracting, obtains the concentrated liquid after cordate houttuynia distillation, standby；Retain the dregs of a decoction after cordate houttuynia steam distillation is extracted, it is standby；
（4）The aqueous solution after honeysuckle flower water steam distillation is extracted is filtered, and is obtained the aqueous solution after honeysuckle distillation, is heated dense Contracting, obtains the concentrated liquid after honeysuckle distillation, standby；Retain the dregs of a decoction after honeysuckle steam distillation is extracted, it is standby；
（5）By step（3）The dregs of a decoction, step after the steam distillation extraction of gained cordate houttuynia（4）Gained honeysuckle flower water steam Distillation extract after the dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, thereto plus 3 times amount 90% alcohol refluxs extractions it is secondary, Refluxing extraction 2 hours, merges ethanol extract every time, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, must mix Ethanol extracts concentrate, standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；
（6）By step（5）The dregs of a decoction after gained ethanol is extracted add 4 times of amount decoctings to boil three times, 2 hours every time, merge water extraction Liquid is taken, is filtered, obtain mixing aqueous extract, heating concentration obtains mixing water and extracts concentrate；
（7）By step（5）Gained mixed ethanol extracts concentrate, step（6）Gained mixing water extracts concentrate, step （3）Concentrated liquid, step after gained cordate houttuynia distillation（4）Concentrated liquid after gained honeysuckle distillation merges, and adds step Suddenly（1）Gained Herba Houttuyniae volatile oil, step（2）Gained volatile honeysuckle oil, mixes, obtains concentrated medicament；
（8）Sucrose is separately taken, simple syrup is made, step is added（7）Gained concentrated medicament, adds water, stirs evenly, and filters, filling, Obtain final product.
Application of the compound houttuynin syrup medicine in treatment tonsillitis medicine is prepared, the compound houttuynin syrup medicine It is by made by the raw material of following weight portion：100 weight portion of cordate houttuynia, 25 weight portion of the root of large-flowered skullcap, 25 weight portion of Radix Isatidis, the capsule of weeping forsythia 10 Weight portion, 10 weight portion of honeysuckle, the compound houttuynin syrup medicine are adopted and are prepared with the following method：
（1）Cordate houttuynia is taken, steam distillation extraction is carried out, Herba Houttuyniae volatile oil is therefrom extracted, it is standby；
（2）Extracting honeysuckle, is carried out steam distillation extraction, therefrom extracts volatile honeysuckle oil, standby；
（3）The aqueous solution after cordate houttuynia steam distillation is extracted is filtered, and is obtained the aqueous solution after cordate houttuynia distillation, is heated dense Contracting, obtains the concentrated liquid after cordate houttuynia distillation, standby；Retain the dregs of a decoction after cordate houttuynia steam distillation is extracted, it is standby；
（4）The aqueous solution after honeysuckle flower water steam distillation is extracted is filtered, and is obtained the aqueous solution after honeysuckle distillation, is heated dense Contracting, obtains the concentrated liquid after honeysuckle distillation, standby；Retain the dregs of a decoction after honeysuckle steam distillation is extracted, it is standby；
（5）By step（3）The dregs of a decoction, step after the steam distillation extraction of gained cordate houttuynia（4）Gained honeysuckle flower water steam Distillation extract after the dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, thereto plus 3 times amount 90% alcohol refluxs extractions it is secondary, Refluxing extraction 2 hours, merges ethanol extract every time, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, must mix Ethanol extracts concentrate, standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；
（6）By step（5）The dregs of a decoction after gained ethanol is extracted add 4 times of amount decoctings to boil three times, 2 hours every time, merge water extraction Liquid is taken, is filtered, obtain mixing aqueous extract, heating concentration obtains mixing water and extracts concentrate；
（7）By step（5）Gained mixed ethanol extracts concentrate, step（6）Gained mixing water extracts concentrate, step （3）Concentrated liquid, step after gained cordate houttuynia distillation（4）Concentrated liquid after gained honeysuckle distillation merges, and adds step Suddenly（1）Gained Herba Houttuyniae volatile oil, step（2）Gained volatile honeysuckle oil, mixes, obtains concentrated medicament；
（8）Sucrose is separately taken, simple syrup is made, step is added（7）Gained concentrated medicament, adds water, stirs evenly, and filters, filling, Obtain final product.
For a better understanding of the present invention, inventor provides following research data, illustrate technique effect of the invention, but under Experiment is stated for further illustrating but being not limited to the present invention.
Experiment one：In compound houttuynin syrup preparation technology, cordate houttuynia is individually extracted and carries the preferred of technique with mixed
First, prescription, process of preparing：
Prescription：Cordate houttuynia 1000g, root of large-flowered skullcap 250g, Radix Isatidis 250g, capsule of weeping forsythia 100g, honeysuckle 100g
Compound houttuynin syrup is prepared by following technique：
Technique one：
（1）Cordate houttuynia is taken, steam distillation extraction is carried out, Herba Houttuyniae volatile oil is therefrom extracted, it is standby；
（2）Extracting honeysuckle, is carried out steam distillation extraction, therefrom extracts volatile honeysuckle oil, standby；
（3）The aqueous solution after cordate houttuynia steam distillation is extracted is filtered, and is obtained the aqueous solution after cordate houttuynia distillation, is heated dense Contracting, obtains the concentrated liquid after cordate houttuynia distillation, standby；Retain the dregs of a decoction after cordate houttuynia steam distillation is extracted, it is standby；
（4）The aqueous solution after honeysuckle flower water steam distillation is extracted is filtered, and is obtained the aqueous solution after honeysuckle distillation, is heated dense Contracting, obtains the concentrated liquid after honeysuckle distillation, standby；Retain the dregs of a decoction after honeysuckle steam distillation is extracted, it is standby；
（5）By step（3）The dregs of a decoction, step after the steam distillation extraction of gained cordate houttuynia（4）Gained honeysuckle flower water steam Distillation extract after the dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, thereto plus 3 times amount 90% alcohol refluxs extractions it is secondary, Refluxing extraction 2 hours, merges ethanol extract every time, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, must mix Ethanol extracts concentrate, standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；
（6）By step（5）The dregs of a decoction after gained ethanol is extracted add 4 times of amount decoctings to boil three times, 2 hours every time, merge water extraction Liquid is taken, is filtered, obtain mixing aqueous extract, heating concentration obtains mixing water and extracts concentrate；
（7）By step（5）Gained mixed ethanol extracts concentrate, step（6）Gained mixing water extracts concentrate, step （3）Concentrated liquid, step after gained cordate houttuynia distillation（4）Concentrated liquid after gained honeysuckle distillation merges, and adds step Suddenly（1）Gained Herba Houttuyniae volatile oil, step（2）Gained volatile honeysuckle oil, mixes, obtains concentrated medicament；
（8）Sucrose is separately taken, simple syrup is made, step is added（7）Gained concentrated medicament, adds water, stirs evenly, and filters, filling, Obtain final product.
Technique two：
Take cordate houttuynia, the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, honeysuckle, plus 7 times of amount decoctings boil 2 times, 2 hours every time, collecting decoction, Filtration, filtrate concentrate the clear cream that relative density is 1.18～1.20, plus ethanol is stirred evenly to alcohol content up to 70%, stands 24 hours, Supernatant is taken, is filtered, decompression filtrate recycling ethanol is simultaneously concentrated, and obtains concentrated medicament；Sucrose is separately taken, simple syrup is made, is added above-mentioned Concentrated medicament, adds water, stirs evenly, and filters, filling, obtains final product.
2nd, evaluation of result method：
With in preparation, the content of Herba Houttuyniae volatile oil is as evaluation index（Detection method reference：Sui Tianshuan, Li Qing, Liu Ran, Deng. the content of 4 kinds of volatile oil in capillary gas chromatography cordate houttuynia. Shenyang Pharmaceutical University journal .2011.28.（2）： 130-134 institutes support method）, the results are shown in Table 1：
1 cordate houttuynia of table is individually extracted and carries the preferred of technique with mixed
3rd, conclusion：In preparation process thereof Herba Houttuyniae volatile oil individually extract the activity that can retain higher in medicinal material into Herba Houttuyniae volatile oil, mixing is divided to extract as the thermal histories Herba Houttuyniae volatile oil volatilization loss such as extraction, concentration, dry is larger, In causing finished product, Herba Houttuyniae volatile oil content is relatively low, therefore using independent extraction process better than in technique for extracting mixed, therefore preparation The technique that cordate houttuynia is extracted using independent steam distillation.
Experiment two：In compound houttuynin syrup preparation technology, honeysuckle is individually extracted and carries the preferred of technique with mixed
First, prescription, process of preparing：
Prescription：Cordate houttuynia 1000g, root of large-flowered skullcap 250g, Radix Isatidis 250g, capsule of weeping forsythia 100g, honeysuckle 100g
Compound houttuynin syrup is prepared by following technique：
Technique one：
（1）Cordate houttuynia is taken, steam distillation extraction is carried out, Herba Houttuyniae volatile oil is therefrom extracted, it is standby；
（2）Extracting honeysuckle, is carried out steam distillation extraction, therefrom extracts volatile honeysuckle oil, standby；
（3）The aqueous solution after cordate houttuynia steam distillation is extracted is filtered, and is obtained the aqueous solution after cordate houttuynia distillation, is heated dense Contracting, obtains the concentrated liquid after cordate houttuynia distillation, standby；Retain the dregs of a decoction after cordate houttuynia steam distillation is extracted, it is standby；
（4）The aqueous solution after honeysuckle flower water steam distillation is extracted is filtered, and is obtained the aqueous solution after honeysuckle distillation, is heated dense Contracting, obtains the concentrated liquid after honeysuckle distillation, standby；Retain the dregs of a decoction after honeysuckle steam distillation is extracted, it is standby；
（5）By step（3）The dregs of a decoction, step after the steam distillation extraction of gained cordate houttuynia（4）Gained honeysuckle flower water steam Distillation extract after the dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, thereto plus 3 times amount 90% alcohol refluxs extractions it is secondary, Refluxing extraction 2 hours, merges ethanol extract every time, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, must mix Ethanol extracts concentrate, standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；
（6）By step（5）The dregs of a decoction after gained ethanol is extracted add 4 times of amount decoctings to boil three times, 2 hours every time, merge water extraction Liquid is taken, is filtered, obtain mixing aqueous extract, heating concentration obtains mixing water and extracts concentrate；
（7）By step（5）Gained mixed ethanol extracts concentrate, step（6）Gained mixing water extracts concentrate, step （3）Concentrated liquid, step after gained cordate houttuynia distillation（4）Concentrated liquid after gained honeysuckle distillation merges, and adds step Suddenly（1）Gained Herba Houttuyniae volatile oil, step（2）Gained volatile honeysuckle oil, mixes, obtains concentrated medicament；
（8）Sucrose is separately taken, simple syrup is made, step is added（7）Gained concentrated medicament, adds water, stirs evenly, and filters, filling, Obtain final product.
Technique two：
Take cordate houttuynia, the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, honeysuckle, plus 7 times of amount decoctings boil 2 times, 2 hours every time, collecting decoction, Filtration, filtrate concentrate the clear cream that relative density is 1.18～1.20, plus ethanol is stirred evenly to alcohol content up to 70%, stands 24 hours, Supernatant is taken, is filtered, decompression filtrate recycling ethanol is simultaneously concentrated, and obtains concentrated medicament；Sucrose is separately taken, simple syrup is made, is added above-mentioned Concentrated medicament, adds water, stirs evenly, and filters, filling, obtains final product.
2nd, evaluation of result method：
With in preparation, the content of volatile honeysuckle oil is as evaluation index（Detection method reference：Su Xiangping, Gong great Chun, Zhang Ya Hero, etc. the research [J] of carbon dioxide supercritical extraction volatile honeysuckle oil chemical composition. when precious traditional Chinese medical science traditional Chinese medicines .2007.18 (11):2643-2644 institutes support method）, the results are shown in Table 2：
2 cordate houttuynia of table is individually extracted and carries the preferred of technique with mixed
3rd, conclusion：In preparation process thereof volatile honeysuckle oil individually extract the activity that can retain higher in medicinal material into Volatile honeysuckle oil, mixing is divided to extract as the thermal histories volatile honeysuckle oil volatilization loss such as extraction, concentration, dry is larger, In causing finished product, volatile honeysuckle oil content is relatively low, therefore using independent extraction process better than in technique for extracting mixed, therefore preparation The technique that honeysuckle is extracted using independent steam distillation.
Experiment three：Compound houttuynin syrup extraction process is preferred
Contain alcohol-soluble active ingredient, and containing water-soluble active ingredient in crude drug used by this preparation.In order to improve original The curative effect of the utilization rate and preparation of material, by prescription drug first with after ethanol extraction, the dregs of a decoction are again with water extraction, such institute for scientific research personnel The active ingredient of extraction is more comprehensive.
Prescription：1000g, root of large-flowered skullcap 250g, Radix Isatidis 250g, capsule of weeping forsythia 100g, honeysuckle 100g
In test, using single factor exploration method, alcohol of the content of active ingredient as index, to gomi herbs with extract Carry, extraction process by water has been carried out preferably.
1. alcohol extraction process is preferred
Contain scutelloside in the root of large-flowered skullcap, be fat-soluble active ingredient.According to its physicochemical property, scientific research personnel with concentration of alcohol, Extraction time is investigation factor, and with alcohol extract, the content of scutelloside goes out optimal alcohol extraction process as performance assessment criteria, preferably.Detection side Method referring to：Wen Huazhen, Xiao Shengyuan, Wang Yiming, Luo Guoan .HPLC methods determine the scutelloside and the Chinese root of large-flowered skullcap of different size Herba Scutellariae scordifoliae Glycosides content [J]. Chinese herbal medicine .2005.36（4）：600-602.It is shown in Table 3, table 4.
3 concentration of alcohol of table it is preferred（Plus 3 times of amounts of alcohol, extract 2 times, every time 2 hours）
4 extraction time of table it is preferred（Plus 3 times of amounts of alcohol, concentration of alcohol is 90%, is extracted 2 hours）
As can be seen from Table 3, in the concentration of alcohol factor that we choose, concentration is the root of large-flowered skullcap in " 90% ethanol " its extract Glycosides content is highest；In table 4, extraction time affects larger to active ingredient, but extracts 2 times with the root of large-flowered skullcap in 3 extracts of extraction Glycosides content is close to, therefore considers from industrial production angle, and selective extraction number of times is " 2 times ".
To sum up, by single factor experiment method, the content of comprehensive active ingredient, we preferably go out alcohol extracting optimised process for " fish Raw meat grass steam distillation extract after the dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, honeysuckle, thereto plus 3 times measure 90% second Alcohol reflux extracts secondary, each refluxing extraction 2 hours ".
2. extraction process by water is preferred
Containing aqueous soluble active constituents such as active ingredient amino acid in Radix Isatidis.According to the property of water soluble ingredient, it is considered to To the cost of actual production, we with water as Extraction solvent, with extraction time as investigate factor, with amino acid content in water extract For performance assessment criteria, Jing single factor experiments show, extracting in water number of times is " 3 times ".Detection method referring to：Ren Guoping, Tian Lu, Lee It is polished, etc. Contents of Amino Acids research [J] in chromatogram of Radix Isatidis. Chinese new drug research .2014,23 (1)：99-105.As a result see Table 5.
5 extraction time of table it is preferred（Add water 4 times and measure, extract 2 hours）
As shown in Table 5, in extract, the content of amino acid increases with increasing for extraction time, 3 extraction amino acid Content highest, still preferably water extraction time be " 3 times ".
3. process summary
Through system research, we show that the optimum extraction process of gomi herbs is：" after cordate houttuynia steam distillation is extracted The dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, honeysuckle, thereto plus 3 times amount 90% alcohol refluxs extract it is secondary, every time Refluxing extraction 2 hours, merges ethanol extract, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, obtains mixed ethanol Concentrate is extracted, it is standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；The dregs of a decoction after above-mentioned gained ethanol is extracted add 4 times of amount water Decoct three times, 2 hours every time, merge aqueous extract, filtration obtains mixing aqueous extract, and heating concentration obtains mixing water and extracts concentration Liquid.”
Experiment four：Extraction process by water is combined with alcohol extracting, water extraction technics comparing
The quality of the technique that combines with alcohol extracting, water extraction for the traditional extraction process by water of comparison, compares experiment.Concrete steps And result is as follows：
First, experimental technique：
Prescription：Cordate houttuynia 1000g, root of large-flowered skullcap 250g, Radix Isatidis 250g, capsule of weeping forsythia 100g, honeysuckle 100g
Compound houttuynin syrup is prepared by following technique：
Technique one：
（1）Cordate houttuynia is taken, steam distillation extraction is carried out, Herba Houttuyniae volatile oil is therefrom extracted, it is standby；
（2）Extracting honeysuckle, is carried out steam distillation extraction, therefrom extracts volatile honeysuckle oil, standby；
（3）The aqueous solution after cordate houttuynia steam distillation is extracted is filtered, and is obtained the aqueous solution after cordate houttuynia distillation, is heated dense Contracting, obtains the concentrated liquid after cordate houttuynia distillation, standby；Retain the dregs of a decoction after cordate houttuynia steam distillation is extracted, it is standby；
（4）The aqueous solution after honeysuckle flower water steam distillation is extracted is filtered, and is obtained the aqueous solution after honeysuckle distillation, is heated dense Contracting, obtains the concentrated liquid after honeysuckle distillation, standby；Retain the dregs of a decoction after honeysuckle steam distillation is extracted, it is standby；
（5）By step（3）The dregs of a decoction, step after the steam distillation extraction of gained cordate houttuynia（4）Gained honeysuckle flower water steam Distillation extract after the dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, thereto plus 3 times amount 90% alcohol refluxs extractions it is secondary, Refluxing extraction 2 hours, merges ethanol extract every time, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, must mix Ethanol extracts concentrate, standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；
（6）By step（5）The dregs of a decoction after gained ethanol is extracted add 4 times of amount decoctings to boil three times, 2 hours every time, merge water extraction Liquid is taken, is filtered, obtain mixing aqueous extract, heating concentration obtains mixing water and extracts concentrate；
（7）By step（5）Gained mixed ethanol extracts concentrate, step（6）Gained mixing water extracts concentrate, step （3）Concentrated liquid, step after gained cordate houttuynia distillation（4）Concentrated liquid after gained honeysuckle distillation merges, and adds step Suddenly（1）Gained Herba Houttuyniae volatile oil, step（2）Gained volatile honeysuckle oil, mixes, obtains concentrated medicament；
（8）Sucrose is separately taken, simple syrup is made, step is added（7）Gained concentrated medicament, adds water, stirs evenly, and filters, filling, Obtain final product.
Technique two：
（1）The mixing of cordate houttuynia, the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia and honeysuckle is taken, plus 4 times of amount decoctings are boiled three times, 2 is little every time When, merge aqueous extract, be condensed into medicinal extract；
（2）Sucrose is separately taken, simple syrup is made, step is added（1）Gained medicinal extract, adds water, stirs evenly, and filters, filling, i.e., .
2nd, evaluation of result method：
With in preparation, the content of Herba Houttuyniae volatile oil, volatile honeysuckle oil, amino acid, scutelloside is as evaluation index, with three The average content of individual composition is comprehensive evaluation index, the results are shown in Table 6.
6 extraction process by water of table is combined with alcohol extracting, water extraction technics comparing result
3rd, conclusion
Compound houttuynin syrup preparation preparation technology retains active component in prescription medicinal material such as higher：Cordate houttuynia is volatilized The scutelloside in volatile honeysuckle oil, the amino acid in Radix Isatidis, the root of large-flowered skullcap in oil, honeysuckle, and traditional extraction process by water preparation Middle active ingredient retention rate is relatively low, it is impossible to ensure the curative effect and quality of medicine, therefore compound houttuynin syrup preparation preparation technology It is advanced compared with traditional handicraft, and have feasibility.
Experiment five：Compound houttuynin syrup treats the experimental study of acute pancreatitis
1 materials and methods
1.1 experiment reagent
Natrium taurocholicum is purchased from Shanghai Ming Rui bio tech ltd；
Compound houttuynin syrup of the present invention：Prescription：Cordate houttuynia 100g, root of large-flowered skullcap 25g, Radix Isatidis 25g, capsule of weeping forsythia 10g, honeysuckle 10g。
Preparation method：
（1）Cordate houttuynia is taken, steam distillation extraction is carried out, Herba Houttuyniae volatile oil is therefrom extracted, it is standby；
（2）Extracting honeysuckle, is carried out steam distillation extraction, therefrom extracts volatile honeysuckle oil, standby；
（3）The aqueous solution after cordate houttuynia steam distillation is extracted is filtered, and is obtained the aqueous solution after cordate houttuynia distillation, is heated dense Contracting, obtains the concentrated liquid after cordate houttuynia distillation, standby；Retain the dregs of a decoction after cordate houttuynia steam distillation is extracted, it is standby；
（4）The aqueous solution after honeysuckle flower water steam distillation is extracted is filtered, and is obtained the aqueous solution after honeysuckle distillation, is heated dense Contracting, obtains the concentrated liquid after honeysuckle distillation, standby；Retain the dregs of a decoction after honeysuckle steam distillation is extracted, it is standby；
（5）By step（3）The dregs of a decoction, step after the steam distillation extraction of gained cordate houttuynia（4）Gained honeysuckle flower water steam Distillation extract after the dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, thereto plus 3 times amount 90% alcohol refluxs extractions it is secondary, Refluxing extraction 2 hours, merges ethanol extract every time, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, must mix Ethanol extracts concentrate, standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；
（6）By step（5）The dregs of a decoction after gained ethanol is extracted add 4 times of amount decoctings to boil three times, 2 hours every time, merge water extraction Liquid is taken, is filtered, obtain mixing aqueous extract, heating concentration obtains mixing water and extracts concentrate；
（7）By step（5）Gained mixed ethanol extracts concentrate, step（6）Gained mixing water extracts concentrate, step （3）Concentrated liquid, step after gained cordate houttuynia distillation（4）Concentrated liquid after gained honeysuckle distillation merges, and adds step Suddenly（1）Gained Herba Houttuyniae volatile oil, step（2）Gained volatile honeysuckle oil, mixes, obtains concentrated medicament；
（8）Sucrose is separately taken, simple syrup is made, step is added（7）Gained concentrated medicament, adds water, stirs evenly, and filters, filling, Obtain final product.
Existing compound houttuynin syrup：Prescription：Cordate houttuynia 100g, root of large-flowered skullcap 25g, Radix Isatidis 25g, capsule of weeping forsythia 10g, honeysuckle 10g。
Preparation method：Take cordate houttuynia, the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, honeysuckle, plus 7 times of amount decoctings boil 2 times, 2 hours every time, Collecting decoction, filtration, filtrate concentrate the clear cream that relative density is 1.18～1.20, plus ethanol is stirred evenly to alcohol content up to 70%, quiet Put 24 hours, take supernatant, filter, decompression filtrate recycling ethanol is simultaneously concentrated, and obtains concentrated medicament；Sucrose is separately taken, simple syrup is made, Above-mentioned concentrated medicament is added, water is added, is stirred evenly, filtered, it is filling, obtain final product.
Yellow Jackets are purchased from Shanghai Jiang Lai bio tech ltd；TNF-α, IL-1 β, the purchase of IL-6 radioimmunological kits From Shanghai Rui Qi bio tech ltd；ICAM-1 rabbit-anti rat proteins immunohistochemical kit is purchased from Wuhan doctor De Sheng Thing Engineering Co., Ltd；NF- κ B p65 rabbit-anti rat proteins immunohistochemical kit is purchased from Beijing Bo Aosen biologies Co., Ltd； Rabbit protein immunization group kit is purchased from Shanghai Ya Ji bio tech ltd.
1.2 animals used as test and packet
Healthy male SD rats, 200, cleaning grade, 1～1.5 month mouse age, 160～200 g of weight, by black dragon River university of TCM Animal Experimental is provided.It is placed in Heilongjiang University of Chinese Medicine's Animal Experimental to raise, keeps clean environment, specially Fed, freely ingest and drunk water with feed, water.Animal is raised 1 week in laboratory adaptability before experiment.Rat acute pancreatitis Model reference literature, driving in the wrong direction for injecting with 5% natrium taurocholicum 1mL/kg pancreatic ducts makes.It is randomly divided into sham-operation group, acute pancreas Adenositis group, acute pancreatitis+compound houttuynin syrup treatment group of the present invention, acute pancreatitis+existing compound houttuynin syrup are controlled Treatment group, totally 4 groups.
Epidural catheter is only inserted and is taken out in pancreatic duct by sham-operation group, not drug；Acute pancreatitis group is model Acute pancreatitis group；After model induction, gavage is of the invention at once for acute pancreatitis+compound houttuynin syrup treatment group of the present invention Compound houttuynin syrup（200mg/kg）1 time, acute pancreatitis+existing compound houttuynin syrup treatment group model induction after, At once the existing compound houttuynin syrup of gavage（200mg/kg）1 time, 50 per group, 40 are respectively taken at random, be divided into 4 time points （3h, 6h, 12h, 24h）, each time point respectively takes 10 and takes serum, then cuts open to kill and takes pancreatic tissue；Another each group rat 10, enters Row Analysis of Survival Time.
1.3 observation indexs and method
1.3.1 each group life span observes survival rate in 72 h of each group.
1.3.2 TNF-α, IL-1 β, IL-6 are determined.
1.3.3 pancreatic tissue histological scores visually observe substantially pancreatic tissue and surrounding pathology situation, take pathology respectively Most heavy sample, using mono blind method, by 2 Pathologis in each organ-tissue pathological change of light Microscopic observation.Pancreas group Knit and scored according to pathological score standard under Schmidt mirrors：Each time point randomly selects the Pancreas pathology section of 3 rats, right Every rat pathological section is individually scored, and the average mark of 3 rats is the last pathological score of each time point pancreas in rat.
1.4 statistical method
All measurement datas mean ± standard deviation（±s）Represent, multiple sample averages of Group Design compare employing One-way ANOAV are analyzed, comparing using Dunnett methods two-by-two between multigroup mean.Count ranked data to examine using sum of ranks Test, P<0.05 thinks that difference is statistically significant.The statistical analysis of whole data are counted using SPSS16.0 software kits Software is analyzed on computers and is completed.
2 results
The life span of 2.1 each group rats
Sham-operation group within observing time without animal dead, the compound houttuynin syrup treatment group surviving rats time of the present invention It is obviously prolonged compared with acute pancreatitis group, difference is statistically significant（P<0.05）, experimental result is shown in Table 7.
The life span of 7 each group rat of table compare (± s, h)
Note：Compare with sham-operation group, * P<0.05；Compare with acute pancreatitis group, #P<0.05
2.2 blood amylases change
Compare with sham-operation group, acute pancreatitis group and the postoperative blood starch of compound houttuynin syrup treatment group rat of the present invention Enzyme becomes apparent rising, statistically significant in each time point difference（P<0.05）；Acute pancreatitis group and compound of the present invention 3 h are raised the blood amylase level of cordate houttuynia syrup treatment group after surgery, are peaked to 6h, are hereafter declined, each time point The blood amylase level of compound houttuynin syrup treatment group of the present invention is below acute pancreatitis group, and difference is statistically significant （P<0.05）, experimental result is shown in Table 8.
The postoperative different time serum amyloid enzymic change of 8 each group rat of table (n=10,± s, U/L)
Note：Compare with time point with sham-operation group, * P<0.05；Compare with time point with acute pancreatitis group, #P<0.05
2.3 serum TNF-cc levels change
Rats in sham-operated group serum TNF-cc level each time point after modeling is without significant change and bright on each time point Aobvious to be less than remaining group, difference is statistically significant（P<0.05）；3h is i.e. obvious after surgery for acute pancreatitis group TNF-α level Rise, 24h reaches peak；The serum TNF-cc level of compound houttuynin syrup treatment group of the present invention is compared with the acute pancreatitis group same time Point（3h, 6h, 12h, 24h）There is substantially reduction（P<0.05）, experimental result is shown in Table 9.
The postoperative different time serum TNF-cc level change of 9 each group rat of table (n=10,± s, ng/mL)
Note：Compare with time point with sham-operation group, * P<0.05；Compare with time point with acute pancreatitis group, #P<0.05
- 1 β levels of 2.4 serum IL change
- 1 β levels of rats in sham-operated group serum IL each time point after modeling is without significant change and bright on each time point Aobvious to be less than remaining group, difference is statistically significant（P<0.05）；3h is i.e. obvious after surgery for acute pancreatitis group IL-1 β Rise, 12h peaks；- 1 β levels of serum IL of compound houttuynin syrup treatment group of the present invention are from postoperative 6h and acute pancreas Scorching group on a declining curve compared with time point, increases over time, and reduces level more obvious.In 3h, 6h, 12h, 24 h sheets Invention compound houttuynin syrup treatment group's each group reduction level has statistics to anticipate with time point comparing difference with acute pancreatitis group Justice（P<0.05）, experimental result is shown in Table 10.
Postoperative -1 β of the different time serum IL changes of 10 each group rat of table (n=10,± s, ng/mL)
Note：Compare with time point with sham-operation group, * P<0.05；Compare with time point with acute pancreatitis group, #P<0.05
2.5 blood serum IL-6 levels change
Rats in sham-operated group serum levels each time point after modeling, without significant change, and is significantly lower than on each time point Remaining two groups, difference is statistically significant（P<0.05）；3 h substantially rise acute pancreatitis group IL-6 after surgery, 12h peaks；The IL-6 of compound houttuynin syrup treatment group of the present invention is same with acute pancreatitis group from postoperative 3h Time point is compared on a declining curve, increases over time, and reduces level more obvious.Treat in compound houttuynin syrup of the present invention The each time points of group 3h, 6h, 12h, 24 h are below same time point acute pancreatitis group, and difference is statistically significant（P< 0.05）, experimental result is shown in Table 11.
The postoperative different time blood serum IL-6 change of 11 each group rat of table (n=3,± s, ng/mL)
Note：Compare with time point with sham-operation group, * P<0.05；Compare with time point with acute pancreatitis group, #P<0.05
2.6 pancreatic tissue histological scores
Have no obvious pathological change under sham-operation group pancreatic tissue mirror, it is compound houttuynin syrup treatment group of the present invention, existing Compound houttuynin syrup treatment group presents different degrees of tissue edema, inflammatory cell infiltration, change with acute pancreatitis group Property the pathological change such as necrosis, but compared with time point, lesion degree mitigates with acute pancreatitis group.Compound houttuynin sugar of the present invention The pathological score of slurry treatment group is compared with time point with acute pancreatitis group, and in 3h, 6h, 12h, 24h difference has statistics to anticipate Justice（P<0.05）, experimental result is shown in Table 12.
The postoperative different time pancreatic tissue pathological score of 12 each group rat of table (n=3,±s)
Note：Compare with time point with sham-operation group, * P<0.05；Compare with time point with acute pancreatitis group, #P<0.05
3 discuss and conclusion
This group treats rat acute pancreatitis using compound houttuynin syrup of the present invention, and treatment group's surviving rats time is more anxious Property pancreatitis group is obviously prolonged, and difference is statistically significant, and pancreatic tissue pathological score is also obviously improved, and shows the present invention Compound houttuynin syrup treatment rat acute pancreatitis have certain curative effect.
The research display of this experimental result, blood amylase in treatment group's serum, TNF-α, IL-1 β, IL-6 levels and acute pancreas Adenositis group compares, and compound houttuynin syrup treatment group of the present invention is less than same time point acute pancreatitis group, poor between two groups of each time point It is different statistically significant（P<0.05）.After prompting compound houttuynin syrup treatment rat model of the present invention, over time Extend, serum inflammatory cytokine TNF-α, IL-1 β, IL-6 levels are reduced compared with acute pancreatitis group, compound houttuynin syrup effectively subtracts The light inflammation of pancreas.
Experiment six：The HPLC finger-prints research of compound houttuynin syrup
The fingerprint analysis method of compound houttuynin syrup is set up using high-efficient liquid phase technique, is to evaluate and control compound fish The method that the quality of raw meat grass syrup provides science.
1 material
1.1 instrument
Waters2695-2998 type high performance liquid chromatographs（The U.S.）；PDA detectors, quaternary gradient pump,
Software is Empower2 data processing software systems；KQ5200DE type numerical control ultrasonic cleaners（Kunshan）. METTLERXS205DU electronic balances（Switzerland）.
1.2 reagent
Compound houttuynin syrup, prepares with reference to the embodiment 1 in description of the invention specific embodiment, is shown in Table by 10 batches 13.Reference substance methyl n-nonyl ketone, β-cubebene, different capsule of weeping forsythia cyclohexanol are purchased from Chinese pharmaceutical biological product calibrating research Institute.Acetonitrile is chromatographically pure, and liquid phase water is Watson distilled water, and it is pure that remaining reagent is analysis.
13 compound houttuynin syrup test sample lot number of table
2 methods and result
2.1 chromatographic condition
Chromatographic column Waters Xbridge C18（4.6mm × 250mm, 5 μm）Post, mobile phase with acetonitrile as mobile phase A, with Water is Mobile phase B, carries out gradient elution, Detection wavelength 203nm, flow velocity 1.0mLmin by table 14-1；30 DEG C of column temperature, sample introduction body 10 μ L of product.
14 mobile phase elution requirement of table
The preparation of 2.2 reference substance solutions
Precision weighs methyl n-nonyl ketone reference substance 4.13mg, β-cubebene reference substance 4.21mg, different capsule of weeping forsythia ring Hexanol reference substance 2.15mg, puts in 10mL measuring bottles, plus methyl alcohol dissolves and be diluted to scale, obtains final product.
The preparation of 2.3 need testing solutions
Above-mentioned S1～S10 compound houttuynins syrup about 0.5g is taken, it is accurately weighed, it is accurate to add methyl alcohol 25mL, weigh, surpass Sonication 30min, takes out, lets cool, and mends weight, shakes up, and filters, takes subsequent filtrate and cross 0.45 μm of filter membrane, obtain final product.
2.4 methodological study
2.4.1 replica test
Same sample lots are taken, precision weighs 6 parts respectively, according to 2.3 lower section legal system available test sample solutions, entered respectively Sample, is that the relative retention time of 1～No. 18 total fingerprint peaks and relative is calculated with reference to peak with No. 4 peak methyl n-nonyl ketones The RSD ＜ 3% of peak area, while the similarity for calculating each chromatographic fingerprinting with similarity evaluation software is all higher than 0.99, show Method repeatability is good.
2.4.2 precision test
Take same need testing solution in replica test, continuous sample introduction 5 times, with No. 4 peak methyl n-nonyl ketones as reference Peak, the RSD for calculating the relative retention time and relative peak area of 1～No. 18 total fingerprint peaks are respectively less than 3%, while with similar Degree evaluation software calculates the similarity of each chromatographic fingerprinting and is all higher than 0.99, shows instrument stabilizer, and precision is good.
2.4.3 stability test
Same need testing solution in replica test is taken, respectively 0,4,8,12,24h sample introductions, with No. 4 peak methyl n-nonyls Ketone is that, with reference to peak, the RSD for calculating the relative retention time and relative peak area of 1～No. 18 total fingerprint peaks is respectively less than 3%, The similarity that each chromatographic fingerprinting is calculated with similarity evaluation software simultaneously is all higher than 0.99, shows need testing solution in 24h It is interior stable.
2.5 the foundation of finger-print
It is accurate draw 2.2 under reference substance solution and 2.3 under each 10 μ L of need testing solution that prepare, inject efficient liquid Chromatography, obtains 10 lot number compound houttuynin syrup HPLC finger-prints, as a result sees Fig. 1.
By the comparison with reference substance, confirm that No. 3 peaks are different capsule of weeping forsythia cyclohexanol, No. 4 peaks are methyl n-nonyl ketone, No. 7 Peak is β-cubebene, wherein No. 4 peak methyl n-nonyl ketone peak areas are larger and more stable, therefore selects this peak to be reference Peak.10 batches of compound houttuynin syrup finger-prints are imported the chromatographic fingerprints of Chinese materia medica similarity recommended using pharmacopoeia commission Evaluation system（A versions）, chromatogram peak match is carried out, matching result is shown in Fig. 2, and gained reference fingerprint is shown in Fig. 3.
With No. 4 peak methyl n-nonyl ketones as reference, after removing solvent peak, determine 18 total peaks to constitute compound fish raw meat The characteristic peak of careless syrup finger-print, the relative retention time and relative peak area at the total peak of sample are listed in table 15 and table respectively 16.10 batches of compound houttuynin syrup are respectively 0.968,0.999,0.998 with reference fingerprint Similarity Measure result, 0.998,0.997,0.990,0.990,0.999,0.999,0.998.15 15 10 batches of compound houttuynin syrup of table of table it is total The relative retention time at peak
The relative peak area at the total peak of 16 10 batches of compound houttuynin syrup of table
3 discuss
Extraction solvent, Detection wavelength, flow phase system are investigated in experiment.Once water, 50% methyl alcohol, 50% second were adopted , used as Extraction solvent, as a result the need testing solution peak shape with water and 50% methyl alcohol as Extraction solvent is not good enough, and separating degree is not high for alcohol, with 50% ethanol is preferable as chromatographic peak peak shape obtained by Extraction solvent, therefore using 50% ethanol as Extraction solvent.
Full wavelength scanner is carried out to collection of illustrative plates using PDAD, as a result the chromatographic peak information under 203nm Compared with horn of plenty, therefore from 203nm as measure wavelength.
Test methanol-water, 2 kinds of flow phase systems of acetonitrile-water during mobile phase condition optimizing respectively, finally choose acetonitrile- , used as mobile phase, chromatographic peak peak shape is preferable with this understanding for water.
Compound houttuynin sugar is determined with methyl n-nonyl ketone, β-cubebene, different capsule of weeping forsythia cyclohexanol to compare peak 18 total peaks of slurry, and the control collection of illustrative plates and each batch of sample of 10 batches of compound houttuynin syrup are obtained by Similarity Measure software With compare the similarity between collection of illustrative plates, be as a result all higher than 0.9, show the stable preparation process of compound houttuynin syrup.Compares figure Spectrum can provide more comprehensive quality control information, can be used as one of quality control and evaluation method of compound houttuynin syrup.
Description of the drawings：
Fig. 1：Compound houttuynin syrup HPLC finger-prints, wherein figure A is reference substance HPLC chromatogram；Figure B is for examination Product HPLC chromatogram finger-print;
Fig. 2：10 batches of sample match chromatograms
Fig. 3：Reference substance finger-print
Specific embodiment：
Embodiment 1：
Prescription：Cordate houttuynia 100g, root of large-flowered skullcap 25g, Radix Isatidis 25g, capsule of weeping forsythia 10g, honeysuckle 10g.
Preparation method：
（1）Cordate houttuynia is taken, steam distillation extraction is carried out, Herba Houttuyniae volatile oil is therefrom extracted, it is standby；
（2）Extracting honeysuckle, is carried out steam distillation extraction, therefrom extracts volatile honeysuckle oil, standby；
（3）The aqueous solution after cordate houttuynia steam distillation is extracted is filtered, and is obtained the aqueous solution after cordate houttuynia distillation, is heated dense Contracting, obtains the concentrated liquid after cordate houttuynia distillation, standby；Retain the dregs of a decoction after cordate houttuynia steam distillation is extracted, it is standby；
（4）The aqueous solution after honeysuckle flower water steam distillation is extracted is filtered, and is obtained the aqueous solution after honeysuckle distillation, is heated dense Contracting, obtains the concentrated liquid after honeysuckle distillation, standby；Retain the dregs of a decoction after honeysuckle steam distillation is extracted, it is standby；
（5）By step（3）The dregs of a decoction, step after the steam distillation extraction of gained cordate houttuynia（4）Gained honeysuckle flower water steam Distillation extract after the dregs of a decoction mix with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, thereto plus 3 times amount 90% alcohol refluxs extractions it is secondary, Refluxing extraction 2 hours, merges ethanol extract every time, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, must mix Ethanol extracts concentrate, standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；
（6）By step（5）The dregs of a decoction after gained ethanol is extracted add 4 times of amount decoctings to boil three times, 2 hours every time, merge water extraction Liquid is taken, is filtered, obtain mixing aqueous extract, heating concentration obtains mixing water and extracts concentrate；
（7）By step（5）Gained mixed ethanol extracts concentrate, step（6）Gained mixing water extracts concentrate, step （3）Concentrated liquid, step after gained cordate houttuynia distillation（4）Concentrated liquid after gained honeysuckle distillation merges, and adds step Suddenly（1）Gained Herba Houttuyniae volatile oil, step（2）Gained volatile honeysuckle oil, mixes, obtains concentrated medicament；
（8）Sucrose is separately taken, simple syrup is made, step is added（7）Gained concentrated medicament, adds water, stirs evenly, and filters, filling, Obtain final product.
Finger-print quality testing：The compound houttuynin syrup of above-mentioned preparation is carried out using following high-efficient liquid phase technique method The quality testing of finger-print, method are as follows：
（1）Chromatographic condition：Chromatographic column Waters Xbridge C18Post, mobile phase with acetonitrile as mobile phase A, with water as stream Dynamic phase B, gradient elution：0min to 12min, mobile phase A are linearly increasing to 30% from 15%, Mobile phase B from 85% linear decline to 70%, 12min to 45min, mobile phase A are linearly increasing to 80% from 30%, Mobile phase B from 70% linear decline to 20%, 45min extremely 55min, mobile phase A are maintained at 80%, and Mobile phase B is maintained at 20%, Detection wavelength 203nm, flow velocity 1.0mLmin-1；Column temperature 30 DEG C, 10 μ L of sampling volume；
（2）The preparation of reference substance solution：Precision weighs methyl n-nonyl ketone reference substance 4.13mg, β-cubebene pair According to product 4.21mg, different capsule of weeping forsythia cyclohexanol reference substance 2.15mg, put in 10mL measuring bottles, plus methyl alcohol dissolves and be diluted to scale, obtains final product；
（3）The preparation of need testing solution：Precision measures 5 mL of compound houttuynin syrup, accurate to add 50% ethanol, 25 mL, 10 min of ultrasonic extraction, 4500 r/min are centrifuged 10 min, and 0.22 μm of miillpore filter filtration takes subsequent filtrate molten as test sample Liquid, obtains final product；
（4）Determine：It is accurate to draw reference substance solution and each 10 μ L injections high performance liquid chromatograph of need testing solution, surveyed It is fixed.
Moreover, it will be appreciated that although this specification is been described by according to embodiment, not each embodiment is only wrapped Containing an independent technical scheme, this narrating mode of specification is only that those skilled in the art should for clarity Using specification as an entirety, the technical scheme in each embodiment can also Jing it is appropriately combined, form those skilled in the art Understandable other embodiment.

Claims (1)

1. a kind of application of compound houttuynin syrup medicine in treatment pancreatitis medicine is prepared, it is characterised in that the compound fish Raw meat grass syrup medicine is by made by the raw material of following weight portion：100 weight portion of cordate houttuynia, 25 weight portion of the root of large-flowered skullcap, Radix Isatidis 25 Weight portion, 10 weight portion of the capsule of weeping forsythia, 10 weight portion of honeysuckle, the compound houttuynin syrup medicine are adopted and are prepared with the following method：
（1）Cordate houttuynia is taken, steam distillation extraction is carried out, Herba Houttuyniae volatile oil is therefrom extracted, it is standby；
（2）Extracting honeysuckle, is carried out steam distillation extraction, therefrom extracts volatile honeysuckle oil, standby；
（3）The aqueous solution after cordate houttuynia steam distillation is extracted is filtered, and obtains the aqueous solution after cordate houttuynia distillation, and heating is concentrated, The concentrated liquid after cordate houttuynia distillation is obtained, it is standby；Retain the dregs of a decoction after cordate houttuynia steam distillation is extracted, it is standby；
（4）The aqueous solution after honeysuckle flower water steam distillation is extracted is filtered, and obtains the aqueous solution after honeysuckle distillation, and heating is concentrated, The concentrated liquid after honeysuckle distillation is obtained, it is standby；Retain the dregs of a decoction after honeysuckle steam distillation is extracted, it is standby；
（5）By step（3）The dregs of a decoction, step after the steam distillation extraction of gained cordate houttuynia（4）Gained honeysuckle flower water steam distillation The dregs of a decoction after extraction are mixed with the root of large-flowered skullcap, Radix Isatidis, the capsule of weeping forsythia, thereto plus 3 times amount 90% alcohol refluxs extract it is secondary, every time Refluxing extraction 2 hours, merges ethanol extract, and filtration obtains mixed ethanol extract, reclaims ethanol and concentrates, obtains mixed ethanol Concentrate is extracted, it is standby；Retain the dregs of a decoction after ethanol is extracted, it is standby；
（6）By step（5）The dregs of a decoction after gained ethanol is extracted add 4 times of amount decoctings to boil three times, 2 hours every time, merge aqueous extract, Filtration, obtains mixing aqueous extract, and heating concentration obtains mixing water and extracts concentrate；
（7）By step（5）Gained mixed ethanol extracts concentrate, step（6）Gained mixing water extracts concentrate, step（3）Institute Obtain the concentrated liquid after cordate houttuynia distillation, step（4）Concentrated liquid after gained honeysuckle distillation merges, and adds step（1） Gained Herba Houttuyniae volatile oil, step（2）Gained volatile honeysuckle oil, mixes, obtains concentrated medicament；
（8）Sucrose is separately taken, simple syrup is made, step is added（7）Gained concentrated medicament, adds water, stirs evenly, and filters, filling, i.e., .
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105168509A (en) * 2015-07-15 2015-12-23 浙江康恩贝中药有限公司 Preparation technology of high-content compound herba houttuyniae mixture
CN105267395A (en) * 2015-11-21 2016-01-27 黑龙江中桂制药有限公司 Compound Yuxingcao syrup extract, compound Yuxingcao syrup and its preparation method

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105168509A (en) * 2015-07-15 2015-12-23 浙江康恩贝中药有限公司 Preparation technology of high-content compound herba houttuyniae mixture
CN105267395A (en) * 2015-11-21 2016-01-27 黑龙江中桂制药有限公司 Compound Yuxingcao syrup extract, compound Yuxingcao syrup and its preparation method

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
RP-HPLC法同时测定复方鱼腥草片中绿原酸、连翘苷、黄芩苷的含量;金永新，等;《中国药师》;20041231;第7卷(第7期);第525页第2.1项 *
复方鱼腥草合剂;国家药品监督管理局编;《国家药品中药标准》;20021231;第231页 *

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